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Volume 87, Issue 1
Displaying 1-19 of 19 articles from this issue
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Michio Nakanishi, Tsuneto Kuriyama, Minoru Oda1967 Volume 87 Issue 1 Pages 1-4
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSMicrodiffusion analysis was successfully applied to the Study of the stability of drugs in solid state. This method is simple and useful to analyze volatile materials formed from drugs by hydrolysis in solid state. It was found by this method thet the decomposition of aluminum aspirin in solid state was a pseudo-zero order process, and the rate constants at each temperature fitted well the Arrhenius' equation. Further, the amount of two kinds of acetic acid, one inherently adsorbed and the other yielded successively by hydrolysis, was found seperately by this mothod.View full abstractDownload PDF (555K) -
Kazue Kondo1967 Volume 87 Issue 1 Pages 5-9
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSMuclear magnetic resonance spectrum of 6-substituted 4, 6-dien-3-one steroids was examined. The olefinic protons showed an interesting shift according to the kind of substituent in the 6-position. The chemical shift of C4-proton was approximately proportional to the magnetic shielding parameter of the substituent in the 6-position. On the other hand, chemical shift of C7-proton was dependent on the mesomeric effect of the C8 substituent and shifts to a higher magnetic field by the presence of an electron-donating group. In the presence of ethoxyl, methoxyl, or fluorine group in the 6-position, which effects the shift of C7-proton to a higher magnetic field, coupling constant (J) was observed between C7-H and C8-H. It was concluded from the fact that the size of J of C7-proton is parallel with the size (+Δδ) of the shift of C7-proton to the higher magnetic field, that the above phenomenon is due not to the steric hindrance of the substituent in the 6-position but rather to the higher electron density in the sp2 at 7-position by the +M effect of the substituent.View full abstractDownload PDF (564K) -
Chiaki Tanaka1967 Volume 87 Issue 1 Pages 10-13
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSIn order to examine the reductive cleavage of aminoxazoles, benzyl 5-phenyl-2-oxazolecarbamate (I), 2-amino-5-phenyloxazole (II), and few related compounds were submitted to catalytic reduction at ordinary pressure, using various catalysts, and following observations were made. 1) I is converted to phenethylurea (IV) via II when using palladium-carbon catalyst in ethanol, and via 1-carbobenzyloxy-3-phenethylurea (VI) when using platinum oxide catalyst. However, II is obtained selectively when using palladium-barium sulfate catalyst in ethanol, and VI, when using platinum oxide catalyst in acetic acid. 2) II affords IV when using either palladium-carbon or platinum oxide catalyst in ethanol or acetic acid. 3) Hydrochloric acid promotes ring cleavage but alkali markedly inhibits fission. 4) Raney nickel is inactive as a catalyst in this reaction. 5) Ring cleavage of ethyl 5-phenyl-2-oxazolecarboxylate (IX) and 5-phenyloxazole (X) do not progress under these conditions.View full abstractDownload PDF (540K) -
Chiaki Tanaka, Hidemi Nishiki1967 Volume 87 Issue 1 Pages 14-21
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSIn order to examine the effect of a substituent on ring fission, benzyl 5-(p-R-phenyl)-2-oxazolecarbamate (I) and 2-amino-5-(p-R-phenyl) oxazole (II) were synthesized, where R was Cl, OH, CH3O, CH3SO2, C6H5, C6H5CH2O, NO2, or NH2. These compounds were submitted to catalytic reduction using palladium-carbon, palladium-barium sulfate, or platinum oxide catalyst. Selectivity of the catalyst and effect of the solvent were approximately the same as those in the case of R=H, as reported in the preceding paper.*1 The substituents present in these compounds were found not to give any marked effect on the ease or difficulty of ring fission.View full abstractDownload PDF (747K) -
Yoshikazu Kondo, Katsuo Hatayama, Toshihiro Ishiguro, Tsunematsu Takem ...1967 Volume 87 Issue 1 Pages 21-26
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSPermanganate oxidation of euphol (I), tirucallol (XII), and β-euphorbol was examined. Permanganate oxidation of I in acetone afforded colorless needles (III), m.p. 224∼225°, C27H44O3, while the same oxidation of β-euphorbol gave yellow needles (VI), m.p. 218∼220°, C27H40O5, besides III. Further oxidation of III with chronic acid in glacial acetic acid afforded yellow needles (VIII), m.p. 178°, C27H38O5. Permanganate oxidation of I in glacial acetic acid afforded VIII, which was also obtained by the same oxidation of β-euphorbol. The same oxidation of XII gives yellow needles (XIII), (efferv. with decomp. at around 215°), C27H40O5. From the nature of the so-called β-euphorbol, it was considered to be a mixed crystal or molecular compound of I and an aldehyde of C10 to C12.View full abstractDownload PDF (662K) -
Yukio Nishimoto, Shyoji Toyoshima1967 Volume 87 Issue 1 Pages 27-32
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSCompounds related to isonicotinic acid hydrazide and their hydrazones show tailing in thin-layer chromatography when using ordinary silica gel. It is considered that this tailing is due to formation of chelate compounds during development by reacting with trace metals in the adsorbent but since the stability of such metal chelates is far smaller than that of organic analytical reagents, this tailing is only weak. In order to prevent this tailing, adsorbent was treated with EDTA and a good result was obtained. Detection of these compounds after development is made by Fe(III)-2, 2'-bipyridyl and by the citric acid reagent solution. Isonicotinic acid hydrazide was detected by the former reagent at above 0.5 μg. Examinations were also made on the separatory detection of related compounds.View full abstractDownload PDF (590K) -
Yoshitaka Mushika, Tadashi Fujita1967 Volume 87 Issue 1 Pages 33-37
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSIn the course of studies on thiamine disulfides, new compounds, thiamine dialkyl phosphate disulfides (III) such as diethyl (IIIa), dipropyl (IIIb), dibutyl (IIIc), and diphenyl (IIId), were synthesized by the oxidation of corresponding thiamine dialkyl phosphate (I) in alkaline solution (method A) and by the dialkyl phosphorylation of thiamine disulfide (IV) with dialkyl phosphorochloridate in pyridine (method B). Oxidation reagents used in method A were iodine, potassium ferricyanide, and hydrogen peroxide. The compounds synthesized by the above two methods were proved to be identical by IR spectra and thin-layer chromatography.View full abstractDownload PDF (556K) -
Yoshiro Usui, Chikashi Matsumura1967 Volume 87 Issue 1 Pages 38-42
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSPhenylpyrazolone derivatives with various halogen substituents were synthesized and relationship between their structure and antifungal activity was examined, using Corticium sasakii. Antifungal activity tended to become weaker in the order of phenylhydrazines, β-acetylphenylhydrazines, phenylhydrazones, and phenylpyrazolones, and with the increasing number of halogens substituted.View full abstractDownload PDF (528K) -
Yoshiro Usui, Chikashi Matsumura1967 Volume 87 Issue 1 Pages 43-65
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSComparative examinations were made on the activities against Piricularia oryzae using the halogen-substituted phenylpyrazolones, halogen-substituted β-acetylphenylhydrazines, and halogen-substituted phenylhydrazines synthesized in earlier work. The activities decreased in the order of hydrazines, acetylhydrazines, and pyrazolones. Assuming that the activity is due to the[chemical formula]skeleton, a series of compounds having this skeleton were synthesized, a total of over 200 compounds classified into 14 groups, and relationship between their structure and activity against rice blast has been discussed.View full abstractDownload PDF (1623K) -
Hyozo Taniyama, Takako Miura, Masahiro Matsuda, Tsunehiro Kitagawa1967 Volume 87 Issue 1 Pages 65-69
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSSynthesis of 2-oxazolidinone derivatives was examined in connection with antituberculous 2, 2'-(ethylenediamino) dibutanol and its starting material, 2-amino-1-butanol. During this work some intermediates were obtained for the synthesis of 2-oxazolidinone derivatives from ethyl chloroformate and α-amino alchol, and their interrelation, especially the state of rearrangement reaction, was clarified.View full abstractDownload PDF (641K) -
Hiroshi Hikino, Kanji Meguro, Genjiro Kusano, Tsunematsu Takemoto1967 Volume 87 Issue 1 Pages 70-74
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSFrom the crude drug "Sen-mokko, " a new sesquiterpenoid, mokko lactone, was isolated and its structure was established as shown in formula I by degradation and spectral evidence. In connection with mokko lactone, dehydrocostus lactone was confirmed to have the structure VIII.View full abstractDownload PDF (683K) -
Toshio Anmo, Mitsunori Washitake, Hiroyuki Shinkai, Tomokazu Suzuki1967 Volume 87 Issue 1 Pages 74-82
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSThe solubility of dequalinium salicylate (I) and dequalinium chloride (II) in water, ethanol, propylene glycol, and combination of these solvents was determined at 0°, 20°, 40°, and 60° by analytical method using ultraviolet absorption. Its results showed that I and II were more easily dissolved in mixed solvents than in individual solvent, and exhibited pronounced maximum solubility in each solvent system. Further, the solubility curves drawn on the triangle diagram indicated that the component of maximum solubility of I and II in mixtures of water, ethanol, and propylene glycol were respectively in a ratio of 25 : 35 : 40, and 15 : 15 : 70.View full abstractDownload PDF (723K) -
Osamu Sakaguchi, Katsushi Yokota, Masuko Suzuki1967 Volume 87 Issue 1 Pages 82-87
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSPurification procedure and chemical properties of glycoprotein in culture filtrate of Asper gillus fumigatus was examined. A glycoprotein was isolated from the culture filtrate by using Sephadex G-50 column, DEAE-Cellulose column, and paper electrothoresis. Chemical properties of the glycoprotein was examined and it contains 95% of carbohydrate which is composed of equimolar amounts of galactose and mannose, with smaller amounts of hexosamine (less than 0.5%) with 0.38% nitrogen and less than 0.1% phosphorus. Amino acid components were eight common amino acids, aspartic acid, glutamic acid, glycine, valine, threonine, phenylalanine, lysine, and arginine.View full abstractDownload PDF (643K) -
Hiroyuki Inouye, Katsuya Tokura, Yuriko Araki1967 Volume 87 Issue 1 Pages 88-94
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSA suitable condition was examined for the preparation of thin layers using a domestic polyamide. Thin-layer chromatography was carried out on domestic and imported polyamides for simple phenols, bromophenols, phenolic tertiary and quaternary alkaloids, and aromatic nitro compounds. The domestic polyamide was found to have better quality among all the samples.View full abstractDownload PDF (676K) -
Toshiyuki Fujii, Tadashi Fujita1967 Volume 87 Issue 1 Pages 95-98
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSThe optical resolution of DL-O-methylserinamide (V), the intermediate in the serine synthesis from acrylonitrile, was described. Resolution of DL-O-methylserinamide (V) was carried out with L-tartaric acid in methanol solution. The precipitated L-hydrogentartrate of L- V, m.p. 172∼173°(decomp.), [α]20D+12.57°(c=1, NHCl), was isolated from the methanol solution, and L-hydrogentartrate of D- V, m.p. 150∼151°(decomp.), [α]20D+0.29°(c=1, NHCl), was crystallized from the mother liquor. Hydrolysis of these optically active V with 47% HBr solution afforded the corresponding L-and D-serine (VI). The synthesized L-serine (VI) was found to correspond to natural serine.View full abstractDownload PDF (525K) -
Seizo Kanao, Tadashi Suyama1967 Volume 87 Issue 1 Pages 99-100
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSDecarboxylation of methylated tertiary amino acid is very difficult but by heating N, N-dimethyl-L-tyrosine (V) in diphenylamine or tetralin at 270°, hordenine (II) was obtained in 35% yield. Tyramine, obtained in 90% yield by decarboxylation of L- tyrosine, was submitted to catalytic reduction over platinum oxide, in the presence of formaldehyde, and hordenine was obtained in 94% yield.View full abstractDownload PDF (358K) -
Masatsugu Matsumoto, Ryoji Murata1967 Volume 87 Issue 1 Pages 101-103
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSPolarographic behavior of aldonolactones was examined using D-arabono-γ-lactone (I), D-galactono-γ-lactone (II), D-glucono-γ-lactone (III), D-glucono-δ-lactone (IV), and D-ribono-γ-lactone (V), as a 1×10-1 M (CH3)4NCl solution (A solution) or 1×10-1 M(CH3)4NCl-3×10-2 M H3BO3 solution (B solution). The half-wave potentials of their reduction wave transited to the negative in I, II, and V, and to positive in III in B solution, while this transition was greatest in higher concentration of H3BO3 with V. These phenomena were considered to be the effect of H3BO3.View full abstractDownload PDF (432K) -
Yoshio Fukui, Kikuko Nakadome, Harumi Ariyoshi1967 Volume 87 Issue 1 Pages 103-105
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSDistribution of taxifolin 3-glucoside (A), taxifolin 3'-glucoside (B), isoquercitrin (C), and d-catechol (D) was examined in the leaves of 28 kinds of Pinaceae Plants, using thin-layer chromatography. It was found that A is a specific component present only in the Chamaecyparis spp., while B is totally absent and C is present in about one-half of the plants examined. Component D was present in all these plants.View full abstractDownload PDF (408K) -
Yasuhito Yamanishi, Nobuyuki Kawasaki1967 Volume 87 Issue 1 Pages 105-107
Published: January 25, 1967
Released on J-STAGE: May 30, 2008
JOURNAL FREE ACCESSSome 2-substituted-3, 5, 6-trimethylpyrazine derivatives were synthesized from 2-chlorotrimethylpyrazine and, by their antibacterial tests, 2-mercapto and 2-(p-nitrophenylsulfonyl) derivatives were found to have antibacterial activities against gram-positive bacteria (Staphylococcus aureus). 2-Sulfanilamido derivative exhibited the same minimum inhibitory concentration against gram-negative bacteria (Eschericherichia coli) as against gram-positive bacteria (Staphylococcus aureus).View full abstractDownload PDF (402K)
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