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Volume 89, Issue 3
Displaying 1-26 of 26 articles from this issue
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SADAO BESSHO, SUIICHI TOMIOKA, SHIRO ITO1969 Volume 89 Issue 3 Pages 291-296
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSSingle compression properties of several substances and their mixtures, and multi-layer compression properties were measured. We propose a presumptive equation to express the compression properties of mixtures and multi-layer compressions, [numerical formula], where Nb is [numerical formula] value when pressure is Pi, Xi, weight fraction in each component, Nbi, [numerical formula] value of each component in the same pressure Pi. This equation seems to approximate the usual type of pharmaceutical tablet compression. The Balshin-type plot, log P=f (Nb), is the most convenient plot type for compression designs.View full abstractDownload PDF (596K) -
TEISUKE OKANO, KAZUYUKI TSUJI1969 Volume 89 Issue 3 Pages 297-301
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSA spectrophotometric study was made on the interaction of the carcinogen 4-nitroquinoline 1-oxide (4-NQO) with nicotinamide, and formation of a charge-transfer complex, in which n-electron of the ring nitrogen of nicotinamide is transferred tothe π-system of 4-NQO was presumed from the following results : (1) A new absorption band characteristic of chargetransfer complex was exhibited in the vicinity of 402 mμ in the difference spectra of aqueous mixtures of nicotinamide and 4-NQO vs. 4-NQO. (2) Analysis of the new absorption band through the Benesi-Hildebrand's equation revealed that a complex of 1 : 1 molar ratio was formed. (3) Intensity of the absorption band decreased in acid region below pH corresponding to pKa of nicotinamide. (4) Intensity of absorption band, which was produced around 396 mμ in the difference spectra of mixed system of 1-methylnicotinamide and 4-NQO was not infiuenced by variation of pH. (5) In the case of mixed system of nicotinamide and 4 -nitropyridine 1-oxide, whose electron affinity is smaller than that of 4-NQO, difference band appeared at about 340 mμ, i.e., in the shorter wave length region than that of the NA-4-NQO system. The magnitudes of ε, K, ΔH, and ΔS values were consistent with the above presumption. Examination of solvent effect revealed that the new absorption bands arose from n→π* transition.View full abstractDownload PDF (634K) -
TEISUKE OKANO, AKIRA TAKADATE1969 Volume 89 Issue 3 Pages 302-309
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESS^1H-nuclear magnetic resonance spectra of 38 kinds of chloro- and fluoro-substituted pyrimidine derivatives at 60 Mcps in deuterated dimethyl sulfoxide, with tetramethylsilane as internal standard, were obtained and examination was made on the relationship between chemical shifts and electron densities computed by simple LCAO-MO method. More or less parallel relationships were found to exist between chemical shifts of 2- and 5-position ring protons and electron densities of carbon atoms at positions 2 and 5, respectively, as well as between 2- and 4-amino protons and 5-methyl protons and electron densities of 2- and 4-amino groups and 5-methyl groups, respectively. It was revealed that electronic influence of substituents on the 5-position proton was larger than that on the 2-position proton. The nuclear magnetic resonance signals of 5-position protons of fluoropyrimidines occurred in higher magnetic field than those of the corresponding chloropyrimidines, which was ascribed to the larger tendency of fluorine atom to donate electrons to the conjugate system than chlorine atom. Examination was made also on the assignment of proton signals of non-equivalent amino groups of 2, 4-diamino-6-chloropyrimidine and 2, 4-diamino-6-fluoropyrimidine, and those in higher magnetic field were assigned to 2-amino protons and those in lower magnetic field to 4-amino protons.View full abstractDownload PDF (780K) -
KUNIHEI INAZU, SHIGEYO SUNAGAWA, RYUICHI YAMAMOTO1969 Volume 89 Issue 3 Pages 310-319
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSAnaerobic degradations of S-alkoxycarbonylthiamines (B1-S-CO-O-R ; R=C2H5 (I), C3H7, iso-C3H7, C4H9, CH2-CH=CH2, CH2C6H5, and CH2CH2C6H5) were studied in aqueous solutions at 100° in a pH range from 1 to 5, and the results were compared with each other and with those of S-benzoyl, S-morpholinocarbonyl, and S-piperidinocarbonyl-thiamines under the same conditions. Each of these B1 derivatives was degraded by a pseudo first-order reaction, and their minimum rates were found to be within a range of pH 2.5 to 3.0. Except for the morpholino- and piperidinocarbonyl compounds, all these derivatives gave B1 and O-alkoxycarbonylthiamine as their thiochrome-reaction-positive products. A correlation was found between the logarithm of the overall rate constants for the degradation of S-alkoxycarbonylthiamines and σ* values for their alkyl groups. An analog computer analysis was made on the degradation of I on the basis of the relative amounts of the degradation products including B1, O-ethoxycarbonylthiamine (XIII), 2-methyl-4-amino-5-hydroxymethylpyrimidine, and 2-methyl-4-amino-5-aminomethylpyrimidine. The results showed that the main degradation route was the transformation of I to a cyclic intermediate which was very easily converted into XIII. Comparisons were made of each rate constant for the other routes with each and with the overall degradation rate constant of I.View full abstractDownload PDF (955K) -
KUNIHEI INAZU, SHIGEYO SUNAGAWA, RYUICHI YAMAMOTO1969 Volume 89 Issue 3 Pages 320-330
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSAnalysis with an analog computer was made on the degradation of O, S-bis (ethoxycarbonyl) thiamine (I) in aqueous solution at 100° in a pH range from of 1 to 5. The analyses were based on both the results of the separate determination of the degradation products including thiamine (B1), O-ethoxycarbonylthiamine (II), S-ethoxycarbonyl thiamine (V), 2-methyl-4-amino-5-hydroxymethylpyrimidine (III), and 2-methyl-4-amino-5-aminomethylpyrimidine (IV), and on the results previously reported for the degradation of II and V. Four different degradation routes of I were found : the two first ones are hydrolyses of -O-COOC2H5 and -S-COOC2H5 to -OH and -SH, respectively, and the other two are direct formations from I to III and to IV. At lower pH values, below or around 1.5, the reaction I→IV proceeded more easily than the other reactions and the reaction I→V was faster than the reaction I→II, where the product V was further converted to II. At the higher pH values, however, the rate of the reaction I→V was small compared with the overall degradation rate of I, and -S-COOC2H5 of I was hydrolysed faster than -O-COOC2H5 of I. These results are supported because we found relative amounts of two different O-alkoxycarbonylthiamines (B1-O-COOR1 and B1-O-COOR2) produced from O, S-bis (alkoxycarbonyl) thiamines (R1-OOC-O-B1-S-COOR2). Furthermore, the stability of I was compared with the stabilities of fifteen different B1 derivatives of acyl, a1koxycarbonyl, and disulfide types in aqueous solutions under the conditions mentioned above.View full abstractDownload PDF (1081K) -
KUNIHEI INAZU, SHIGEYO SUNAGAWA, RYUICHI YAMAMOTO1969 Volume 89 Issue 3 Pages 331-335
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSComparative studies were made on the stabilities of ethoxycarbonylthiamines, benzoylthiamines, and related thiamine derivatives in aqueous solutions of pH 7.4 at 37.4°. Each of these compounds was degraded by a pseudo-first-order reaction. The time necessary for a 10% decrease in the residual fraction was 12.5 hours for O-ethoxycarbonylthiamine, 0.66 hours for S-ethoxycarbonylthiamine, and 87.1 hours for O, S-bis (ethoxycarbonyl) thiamine. Comparison of these values with those of other compounds is shown in Table I. Of the derivatives having one or more substituents of the same type, an S-monosubstituted derivative was the least stable, followed by the O-monosubstituted, and the O, S-disubstituted compound was the most stable. Both the S-ethoxycarbonyl- and S-benzoyl-thiamines were easily converted into thiamine. The major part of O-ethoxycarbonyl-, and O-benzoyl-thiamines was decomposed to thiochrome reaction-negative compounds, and minor amounts were hydrolysed to thiamine. Parts of disubstituted derivatives were hydrolysed to thiamine and the corresponding thiamine-O-ester, the latter of which resulted mainly from the cleavage of the thioester linkage. When the period of storage was extended beyond about 30 days for thiamine disulfide and about 85 days for thiamine propyl disulfide, the residual fractions decreased markedly, showing a deviation from the pseudo-first-order character.View full abstractDownload PDF (546K) -
SHUJIRO GOYA, HIROSHI HOSODA, TOSHIHIRO KUDO, CHITOSHI ANZO, TOSHIO NA ...1969 Volume 89 Issue 3 Pages 336-339
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSPolarographic reductions of seven pairs of epimeric a-bromo-17- and -16-ketosteroids were carried out in isopropanol-acetate buffer solution (pH 6.0) (4 : 1) and the relationship between the half-wave potentials and the nature of C-bromine bond was examined on the basis of stereochemical and conformational grounds (Table I). There could be seen the difference in the half-wave potential between each epimer of a-bromoketones ; and the thermodynamically less stable epimer was reduced with more ease than the other one. In addition the reduction of these compounds at the dropping mercury electrode was also influenced by the change of C/D-ring fusion and slgihtly by the structural alteration of ring A and B.View full abstractDownload PDF (505K) -
HARUO SAIKACHI, KEIJI TAKAI1969 Volume 89 Issue 3 Pages 340-344
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSOlefination of 14 kinds of furan system carbamoylmethylenetriphenylphosphoranes (Ia to IVb) and 5-nitro-2-furfural (VI) was attempted but objective compounds were not obtained from any of them. Reaction of four kinds of phenylcarbamoylmethylenetri-phenylphosphoranes (Va to Vd) with VI gave the objective amido olefin compound (VIIIa) alone from Va, VIIIb and a by-product olefin compound (IXb) from Vb, IXc, VIIIc, and the betaine compound (VIIc) of the latter from Vc, and only IXd from Vd. Formation mechanism of the olefins (IXb to IXd) was assumed to involve thermal dissociation of Vb to Vd.View full abstractDownload PDF (548K) -
YASUHIKO SASAKI, JUUKOU SUGIHARA, AKIRA WATANABE, MARI SAKUMA, MINEZO ...1969 Volume 89 Issue 3 Pages 345-353
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSThe distribution, excretion and metabolism of 1-methyl-3-[bis(2-thienyl)methylene] piperidine (I) in the rat were studied by colorimetric and radiochemical methods. It was found that I was well absorbed from the digestive tract and quickly metabolized in the liver. Immediately after the intravenous injection of tritiated I, radioactivity was the highest in the lung, relatively high in the brain, and very low in blood. Most of the radioactivity in the lung and brain was due to unchanged tritiated I, and that in the liver was due to many other radioactive metabolites. About 70% of the radio activity after the intravenous injection of tritiated I was recovered from 24 hours feces and urine, and 50% was recovered after its oral administration. Most of the radio activity in urine was due to radioactive metabolites and the amount of unchanged tritiated I and its N-demethylated compound (II) was very small. Some of the metabolites were found to be glucuronic acid conjugates but none of their aglycones were I or 3-[di(2-thienyl)methylene]piperidine hydrochloride (II). About 4% of the administered radioactivity after intraperitoneal injection of 14C -labeled I was expired as 14CO2 in 24 hours, and most of 14CO2 was expired in the first 3 hours.View full abstractDownload PDF (946K) -
HIDEOMI FUKUDA, KAZUO WATANABE, NOBUKO NAKAMURA, CHIZUKO HOSHINO, KOJI ...1969 Volume 89 Issue 3 Pages 354-358
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSSeventeen ammonium salts of fluorine-substituted benzhydryl aminoethyl ethers were synthesized and pharmacological properties of fifteen compounds were examined. Several compounds were found to suppress the tremor caused by harmine in mice. A dose of 30 mg/kg of 2-morpholinoethyl p-fluorobenzhydryl ether methylbromide (V) or 2-(1-pyrrolidinyl) ethyl p-chlorobenzhydryl ether methyliodide (IX) injected intraperitoneally had a more potent anti-harmine activity than the same dose of diphenhydramine, suggesting expectations of the drugs being active for Parkinsonism. Antihistaminic and anti-acetylcholine activities of the tested compounds in vitro were weaker than those of diphenhydramine and atropine respectively. As to the muscle relaxant activity, these compounds (1×10-5 g/ml) decreased acetylcholine (1×10-5)-induced contraction of frog rectus by 60 to 90%, and 1×10-5 to 3×10-5 decreased the twitches of the isolated frog sartorius elicited by nerve-stimulation. In the case of the whole animal however, intraperitoneal injection of 50 mg/kg of these compounds to mice did not show any remarkable sign.View full abstractDownload PDF (671K) -
TOSHIO ANMO, MASAHARU NARITOMI, HIROJI ONO, MASAMICHI ASANO1969 Volume 89 Issue 3 Pages 359-364
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSIn the present report, relaxation rate constant k, which is the reciprocal of relaxation time, has been evaluated in order to investigate the compression mechanism of powder. Microcrystalline cellulose powder obtained by crushing the tablet compressed at the pressure 3000 kg/cm2 is used as sample (SA) in the experiment. The hardness of SA tablet is lower than that of the tablet of microcrystalline cellulose (A) without any treatment at the same compression pressure. In order to explain the above difference the relaxation rate constant k of SA to the applied pressure was discussed in comparison with the case of A. As the results, it is revealed that the plastic property disappears in the pressure range of 500 to 1200 kg/cm2 and that the structure-fixed state which was introduced in the previous report is rather unstable in the pressure range of 1200 to 2200 kg/cm2. The SA rate constant k remains at low value in the pressure range of 2200 to 2800 kg/cm2, where the decrease of hardness seems to be due to strain recovery. It is that displacement, relative density and hardness are governed by the rate constant k. This result is consistent with that of the previous report.View full abstractDownload PDF (883K) -
HIROYUKI SHINKAI1969 Volume 89 Issue 3 Pages 365-371
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSThis report describes on in vitro method that allows to study the percutaneous absorption through the human excised skin of hydrocortisone-4-14C and hydrocortisone acetate-4-14C diluted in various liquid vehicles. The excised skin was bound to the apparatus as shown in Fig. 1. The radioactivity in the skin surface residual and in the saline layer was counted by liquid scintillation method. The radioactivity in the skin was exchanged to 14CO2 in oxygen flask, and then counted in a liquid scintillation counter using hyamine 10X (1M methanol solution). The results showed that the amount of hydrocortisone acetate released in skin from the liquid vehicles is about 0.1 to 0.5 per cent. The release of hydrocortisone was less than its acetate. Radioactivity in saline layer was not detected in all cases.View full abstractDownload PDF (749K) -
HIROSHI HIKINO, CHOHACHI KONNO, TSUNEMATSU TAKEMOTO1969 Volume 89 Issue 3 Pages 372-374
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSA new phenolic glycoside pleoside (I) was isolated from the whole plant of Pleopeltis thunbergiana. Hydrolysis of I with dil. sulfuric acid gave glucose and a phenolic aglycone (II) which afforded a monomethyl ether (III) by treatment with diazomethane. II and III were established, by spectral data, as 2, 6-dihydroxy-4-methoxyacetophenone and 2-hydroxy-4, 6-methoxyacetophenone, respectively. The above evidence together with the enzymatic hydrolysis and the molecular rotation of I indicate that I is 2, 6-dihydroxy-4-methoxyacetophenone 2-β-D-glucopyranoside.View full abstractDownload PDF (417K) -
SANYA AKABOSHI, TERUO KUTSUMA1969 Volume 89 Issue 3 Pages 375-381
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSThe ultraviolet absorption spectra of 2', 4'-dihydroxychalcone (V), 4'-(benzyloxy)-2'-hydroxychalcone (VI) and azachalcones (Ila-c, IIIa-c) corresponding to V and VI are reported. These chalcones and azachalcones show two absorption maxima in the wavelength region over 280 mμ, λ1 (345-350 mμ) and λ2 (282 -324 mμ) respectively. It was confirmed that λ1 is due to the electronic nature of the conjugation system of dihydroxybenzoyl group (IA) and λ2 is due to that of cinnamoyl group (IB). Relations between the values of λ1 and λ2, and the position of nitrogen atom in the azachalcones were also discussed.View full abstractDownload PDF (667K) -
HIDEOMI FUKUDA, KAZUO WATANABE, TSUGUTAKA ITO1969 Volume 89 Issue 3 Pages 382-388
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSA study was made to clarify the mechanisms of amyostatic action of Lyoniol-A isolated from Lyonia ovalifolia var. elliptica. In the intact mice, intraperitoneal injection of 5 mg/kg of Lyoniol-A caused postures characterized by torsion, retrocollis, spasm, and locomotive ataxia. These postures were also observed in rats, chicks, and frogs. Lyoniol-A in a concentration of 5×10-6 g/ml did not alter the twitches of both isolated frog sartorius muscle and rat diaphragm elicited by a nerve stimulation. Intravenous injection of 1 mg/kg of Lyoniol-A produced contraction of the guinea-pig ileum in situ, whereas 5×10-6 g/ml of it did not have any effect on the responsiveness of the isolated Guinea-pig ileum, suggesting that the autonomic response to Lyoniol-A was via the central nervous system. A small dose of Lyoniol-A injected intraventricularly produced an immediate effect in mice. In the intact chicks as well as in the spinal ones, Lyoniol-A slightly enhanced the crossed extensor reflex. In evoked electromyogram in chicks, intravenous injection of 2 mg/kg of Lyoniol-A induced late responses, which seemed to be due to the interference with spinal and supraspinal structures. From these results the possible mode of action of Lyoniol-A is discussed.View full abstractDownload PDF (1092K) -
YOSHIO ARATA, TOMIKO SHIODA, JUNKO YAMADA, YASUKO HAYASHI1969 Volume 89 Issue 3 Pages 389-391
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSCatalytic reduction of ethyl 2-ethoxycarbonyl-4- (2-pyridyl) butanoate (I) over platinum·rhodium followed by distillation led to III which, on heating with barium hydroxide, gave V in good yield. The action of N-bromosuccinimide on VI derived from V afforded IX. An N-oxide (X) derived from VI was warmed in a tartaric acid solution containing ferric nitrate to give VIII and IX.View full abstractDownload PDF (479K) -
YOSHIHISA ARAI, KINGO ENOMOTO1969 Volume 89 Issue 3 Pages 392-398
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSEffect of two 1-alkyl substituted isoquinoline derivatives, having antitumor activities, on energy-generating system of Ehrlich ascites carcinoma cells and normal hepatic cells was investigated. 1-(2-Methylbutyl)-3-methyl-6, 7-methylenedioxyisoquinoline hydrochloride (B-15) and 1-(1, 1-dimethylpropyl)-3-methyl-6, 7-methylenedioxyisoquinoline hydrochloride (B-19) were strong inhibitiors of dehydrogenase activities of these cells in the medium free from any substrate. However, when glucose was used as a substrate, B-19 was stronger inhibitor of dehydrogenase activities of Ehrlich ascites carcinoma cells than B-15. Both compounds showed marked inhibitory effect on endogenous respiration of the cells, and especially a selective inhibitory activity against Ehrlich ascites carconoma cells was observed with B-15. However, oxygen consumption of Ehrlich ascites carcinoma cells respiring in the presence of glucose was stimulated with an optimum concentration of B-15, whereas anaerobic glycolysis of the cells was inhibited by these compounds when the production of lactate was measured. From these results, it was suggested that these compounds might have a different effect on the respiration of the cells.View full abstractDownload PDF (787K) -
SADAO BABA, SHOZABURO OGIYA1969 Volume 89 Issue 3 Pages 399-402
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSA method of separatory determination of aliphatic primary amines excreted in human urine was established with the amino acid analyzer, This method was applied to the determination of aliphatic primary amines in the distillate of amine concentrate prepared from urines of normal persons and patients. It was clarified that urinary excretion of ethanolamine and methylamine increased in liver diseases but remarkably decreased in kidney diseases. No difference was observed in diabetes mellitus as compared with normal persons. n-Propylamine and isopropylamine detected qualitatively by thin-layer chromatography by others were not found in our experiments.View full abstractDownload PDF (470K) -
KENJI SHIMADA, YUZO NAGASE, USHIHO MATSUMOTO1969 Volume 89 Issue 3 Pages 403-409
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSd-Dethiobiotin tritiated at selective positions can be prepared by reductive desulfurization of d-biotin with Raney nickel catalyst. Three combinations of the solvent (water) and the catalyst (Raney nickel) were examined as follows : 1) Tritiated water and ordinal Raney nickel (W-2) 2) Tritiated water and 3H2 gas-adsorbed Raney nickel 3) Non-labeled water, and Raney nickel adsorbed with tritium gas. Although d-dethiobiotin was labeled with tritium by any of these combinations, labeled products with high specific radioactivity were obtained with 3H2-adsorbed Raney nickel in 2) and 3). In order to clarify whether the tritium incorporated into 3H-d-dethiobiotin is derived from tritium water or 3H2-adsorbed catalyst, the tritiation mechanisms were investigated. Tritium atoms were shown to be freely interchangeable between the solvent (3H2O) and the catalyst (3H2-adsorbed Raney nickel) during the catalytic desulfurization of d-biotin. The tritiated d-dethiobiotin obtained was assumed to be predominantly 5-methyl[3H]-2-oxo-4-imidazolidinehexanoic [6-methylene-3H] acid from infrared and nuclear magnetic resonance data of 2H-d-dethiobiotin prepared by the reductive deuterization of d-biotin using an analogous method.View full abstractDownload PDF (756K) -
TSUYOSHI TOMIMORI, MANKI KOMATSU1969 Volume 89 Issue 3 Pages 410-417
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSWe previously reported that norswertianin (I), swertianin (II), methylswertianin (IV), desmethylbellidifolin (VI), and bellidofolin (VII) were isolated from the whole herb of Swertia japonica MAKINO (Gentianaceae).1) Besides these compounds, methylbellidifolin (IX) has now been isolated and identified. At the same time, xanthone constituents were examined in six different kinds of Swertia SPP., the results are shown in Table II. A C-glucoside of Swertia chirata BUCH.-HAM. was identified as mangiferin (XI) from its physical properties and its ability to give norathyriol (XII) by action of hydriodic acid. In addition, the "swertianolin" structure was revised as being now a 1-O-glucoside of bellidifolin (X).View full abstractDownload PDF (960K) -
TETSUJI KAMETANI, KAZUO KIGASAWA, HIROSHI SUGAHARA, MINEHARU HIIRAGI, ...1969 Volume 89 Issue 3 Pages 418-421
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSIn the previous paper we have assumed that 3-amino-4-oxoisocarbostyril (V) would be formed during catalytic hydrogenation of 3-oximino-4-oxoisocarbostyril (III) in the presence of hydrochloric acid, but, after various examinations, the compound (V) was found to be 3-carbamoylphthalimidine (VI) formed by the ring contraction of III. Furthermore, acid hydrolysis of VI afforded an acid (VII), whose IR spectrum (in KBr) was not identical with that of the product obtained by alkaline hydrolysis of VI. In this case the IR (in dioxan) and NMR spectra of VII and hydrolytic product of VI were completely identical. The crystalline form of VII varies according to the solvent of recrystallization. These facts show that the two forms of crystals would be dimorphic.View full abstractDownload PDF (441K) -
TSUKINAKA YAMANA, YUZO MIZUKAMI, AKIRA TSUJI1969 Volume 89 Issue 3 Pages 422-425
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSThe influences of the solvents on the rate constants were investigated for the degradation of chlorothiazide (I) in phosphate buffer solutions (pH 7.9, μ=0.1) at 87.5°. The specific rate constants decrease with increasing concentrations of organic solvents (ethanol, n-propanol, propylene glycol, acetone, dioxane) down to 10-20%. A slight increase of the specific rate constants occurs at higher solvents concentration. The results are not in agreement with the Laidler's electrostatic theory.View full abstractDownload PDF (431K) -
KIYOSHI TAKIURA, MINORU YAMAMOTO, SHIGEKO OHKAWA1969 Volume 89 Issue 3 Pages 426-429
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSAldotetronolactone forms a complex salt with molybdic acid and the optical rotation of the former at D line changes with complex formation. The rate at which this optical rotation reaches equilibrium is the fastest at pH 6 and a constant maximum value is reached after 24 hours. As a result of measurement by the continuous variation method and molar ratio method, binding ratio of aldotetronolactone to molybdic acid was found to be 2 : 1. Measurement of optical dispersion of the complex salt formed by the addition of molybdic acid to aldotetronolactone showed that the maximum rotations is present at 330 mμ in any of the lactones. Drude's monomial corresponding to these curves was calculated. The empirical rule of Okuda and others established between the sign of the Cotton effect and hydroxyl in 2-position of the lactone can also be applied to aldotetronolactone.View full abstractDownload PDF (444K) -
TADAHIRO NARAFU1969 Volume 89 Issue 3 Pages 430-431
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSIn the previous works of this series, 1, 3) it was found that (2-bromoacyl) ureides administered orally were excreted as the corresponding debrominated metabolites in the urine of rabbits. The present investigation was undertaken in order to determine whether these metabolites were also found in the urine when the drugs were administered subcutaneously to rabbits at the dose of 100 mg/kg body weight. As the results, we found almost same amount of, debrominated metabolites as in the case of oral administrtion described in the previous paper, 1, 3) and therefore it was concluded that most of the metabolites produced in vivo was not attributable to the action of intestinal bacteria.View full abstractDownload PDF (356K) -
NOBUHIKO IRITANI, TAKETSUNE MIYAHARA, ICHIRO TAKAHASHI1969 Volume 89 Issue 3 Pages 432-435
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSDiphenehydramine hydrochloride, chlorphenylamine maleate, thonzylamine hydrochloride, promazine hydrochloride, procaine hydrochloride, papaverine hydrochloride, quinine hydrochloride, and atropine sulfate were precipitated with Reinecke salt. Chromium (III) in the precipitation was determined by chelatometry. When 3-15 mg of the base was treated, the error was less than ±0.5%. The recommended procedure is as follows : Ten mililiter of the sample solution, 5 ml of 20% sulfuric acid, and 5 ml of 1% Reinecke salt solution are mixed. After standing for 1 hour, the precipitate is filtered on a glass filter, washed with cold water, and dissolved in small portion of dimethylformamide. The solution is mixed with 5-10 ml of 0.01M EDTA solution and acetate buffer (pH 4), after boiling 10 minutes, titrated fluoro-photometrically with 0.01M copper sulfate solution using calcein as the indicator. Determination of the organic bases in powder was discussed.View full abstractDownload PDF (457K) -
KENJI SHIMADA, YUZO NAGASE, USHIHO MATSUMOTO1969 Volume 89 Issue 3 Pages 436-440
Published: March 25, 1969
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSThe isotope dilution method for the determination of d-biotin was investigated. d-Biotin reacted with p-dimethylaminocinnamaldehyde (p-DACA) to develop intense coloration having an absorption maximum at 533 mμ, which can be used for colorimetric determination. The conditions for color development were examined. Radioactivity measurements were simultaneously made by using aliquots of the colored solution. d-Biotin tritiated by the Wilzbach method was used as a tracer. d-Biotin was separated by thin-layer chromatography, and isolated with absolute ethanol. The extracts were dehydrated with anhydrous sodium sulfate, and color was developed by addition of p-DACA. After allowing it to stand for one hour, absorbancy and radioactivity were measured, and the recovered specific radioactivities were calculated. The proposed isotope dilution analysis gave the d-biotin in 99.4-101.8% recovery. The method was applied for commercialized d-biotin-containing preparations (injections and tablets). Compared with microbioassay, the above described isotope method has some merits in a rapid microscale determination of d-biotin quantitatively. This method may be widely applicable for the specific determination of d-biotin from biotin related compounds (biotin sulfoxides and biocytin etc.) in biological materials.View full abstractDownload PDF (558K)
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