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Volume 106, Issue 3
Displaying 1-14 of 14 articles from this issue
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Thermal Solid-State Reactions and Mechanochemical Effects of 1-Methyl-4-oxo-cis-2, 6-diphenylthianium Tetrafluoroborate with Alkali HalidesKENJI TOKUNO, YUKARI ASAO, FUMIHISA MIYOSHI, YUKIE SAWADA, TSUTOMU OHA ...1986 Volume 106 Issue 3 Pages 187-192
Published: March 25, 1986
Released on J-STAGE: January 31, 2011
JOURNAL FREE ACCESSIn the solid state, a characteristic reaction is observed on heating of ground mixtures of 1-methyl-4-oxo-cis-2, 6-diphenylthianium tetrafluoroborate (1) and alkali halides. These reactions occurred via ion exchange. These reaction products were 4-oxo-cis-2, 6-diphenylthiane (6) and 5-(methylthio)-1, 5-diphenyl-(E)-1-penten-s-trans-3-one (3) in KC1, mainly dibenzalacetone (4) in KBr, 1, 5-bis (methylthio)-1, 5-diphenylpentan-3-one (5), 3, 4, and 6 in KI, 3, 4, and 6 in NaCI, respectively, and different from those at room temperature. Moreover, the existence of three crystal forms (form I, II and III) and an amorphous form of 1 was confirmed by powder X-ray diffraction. Polymorphic transformations caused by heating, standing and by mechanical treatment such as grinding. In the solid-state reaction, grinding of mixture occurs the interaction such as adsorption. Moreover, thermal solid-state reaction by differential thermal analysis was affected by the grinding times and amount of alkali halide.View full abstractDownload PDF (950K) -
Solid-State Reactions of 1-Methyl-4-oxo-trans-2, 6-diphenylthianium Tetrafluoroborate with Alkali HalidesKENJI TOKUNO, YUKARI ASAO, FUMIHISA MIYOSHI, YUKIE SAWADA, TSUTOMU OHA ...1986 Volume 106 Issue 3 Pages 193-198
Published: March 25, 1986
Released on J-STAGE: January 31, 2011
JOURNAL FREE ACCESSThe solid-state reaction of ground mixture of 1-methy1-4-oxo-trans-2, 6-diphenylthianium tetrafluoroborate (2) with some alkali halides (AX) has been investigated. In each system, an ion exchange reaction between 2 and AX occurred followed by the S-C bond cleavage in oxothianium ion. At room temperature, the ground mixture of 2 with KCl, KBr or NaCl gave 5-(methylthio)-1, 5-diphenyl-(E)-1-penten-s-trans-3-one (3) and with KI gave 4-oxo-cis-2, 6-diphenylthiane (5) in quantitative yield, respectively. When the ground mixtures were heated, the product was 3 in KCl and dibenzalacetone (6) in KBr, quantitatively. The products were 3 and 6 in NaCl and 3, 5, 6 and 1, 5-bis (methylthio)-1, 5-diphenylpentan-3-one (7) in KI. On heating system, activated hydrogen halide gas gencrated by the β-elimination reaction attacked 3 and produced 6. Stereomutation at C2 or C6 of oxothianium ion was observed accompanied by the ion exchange both in NaCl and KI media. It is considered that these stereomutation occurredviapyramidal inversion at the sulfonium carbanion.View full abstractDownload PDF (1012K) -
Fractionation and Purification of Antitumor Polysaccharide H11HISANORI KANAYAMA, NORIHIKO ADACHI, YOSHIKAZU FUKAI, IKUE TAKEUCHI, MA ...1986 Volume 106 Issue 3 Pages 199-205
Published: March 25, 1986
Released on J-STAGE: January 31, 2011
JOURNAL FREE ACCESSA polysaccharide mixture, fraction A, was extracted from the mycelia of Poria cocos (SCHW.) WOLF with 1 N KOH solution and precipitated with ethanol. Fraction A showed a strong antitumor effect against implanted sarcoma 180 (solid type) in mice. Fraction A was fractionated into two fractions F1 ([α]D26+120°) and F2 ([α]D26+170°) by salting out with ammonium sulfate and subsequently by DEAE-Sephadex A-25 column chromatography. Furthermore, the antitumor active fraction F1 was separated into three fractions H11, H12 and H2 by affinity chromatography by use of Con A-Sepharose. Of these three fractions, only fraction H11, homogeneous on electrophoresis, showed a strong antitumor effect. On complete hydrolysis, fraction H11 gave D-glucose as a sole product. It is suggested that the glucosidic linkage in fraction H11 has a β-configuration from the negative low specific rotation ([α]D26-28.2°) and absorption at 890cm-1 in the infrared spectrum.View full abstractDownload PDF (855K) -
Structural Analysis of Antitumor Polysaccharide H11HISANORI KANAYAMA, NORIHIKO ADACHI, YOSHIKAZU FUKAI, IKUE TAKEUCHI, MA ...1986 Volume 106 Issue 3 Pages 206-211
Published: March 25, 1986
Released on J-STAGE: January 31, 2011
JOURNAL FREE ACCESSStructural analysis was made on the glucan moiety of purified antitumor active polysaccharide fraction H11 obtained from the mycelia of P. cocos.
In the 13C-nuclear magnetic resonance spectrum of fraction H11, signals at 102.9 and 84.8ppm were observed, and assigned to C-1 of the β-linkage and C-3 of the β-D-(1, 3)-linked D-glucosyl redidues, respectively. On addition of NaOD solution, the C-1 signal was separated into two signals at 104.2 and 104.8ppm which can be assigned to the C-1 signal of the β-D-(1, 3)-linked and the β-D-(1, 6)-linked D-glucosyl residues, respectively.
The molecular weight of fraction H11 was calculated to be approx. 5×106 by the gel filtration method with CPG-1000Å.
Complete methylation and hydrolysis of fraction H11 gave 2, 4, 6-tri-, 2, 3, 4-tri-, 2, 4-di-, and 2, 3, 4, 6-tetra-0-methyl glucose as alditol acetates in a molar ratio of 3.96: 0.95: 1.05: 1.00.
From these results, it has been revealed that fraction H11 is a highly branched (1, 3)-(1, 6)-β-D-glucan containing each component in 4: 1 ratio.View full abstractDownload PDF (721K) -
HIROTAKA SHIBUYA, MINORU YOSHIHARA, EISAKU KITANO, MASAKAZU NAGASAWA, ...1986 Volume 106 Issue 3 Pages 212-216
Published: March 25, 1986
Released on J-STAGE: January 31, 2011
JOURNAL FREE ACCESSThe essential oil constituents in Zedoariae Rhizoma (Gajutsu in Japanese) originated in China, Taiwan, and Yakushima (Japan) were analyzed by means of gas liquid chromatography-mass spectrometry (GC-MS) by using hitherto elucidated nine sesquiterpenoids (1-9) as standard substances. Each essential oil gave a characteristic reconstructed ion current chromatogram as shown by the qualitative analysis and the essential oil composition of Rhizoma from Yakushima was shown to be a sum of the essential oil compositions of Rhizoma from China and Taiwan. The major sesquiterpenoid of each essential oil was shown by the quantitative analysis as furanogermenone (8) in Rhizoma from China, curcumenol (6) in Rhizoma from Taiwan, or dehydrocurdione (4) in Rhizoma from Yakushima (Japan).View full abstractDownload PDF (749K) -
SATOSHI KOBAYASHI, KATSUMI TAKAI, AKINOBU INOUE1986 Volume 106 Issue 3 Pages 217-220
Published: March 25, 1986
Released on J-STAGE: January 31, 2011
JOURNAL FREE ACCESSA high performance liquid chromatographic procedure has been developed for the determination of flunarizine in biological materials. Flunarizine and the internal standard (cinnarizine) were extracted from alkalinized biological fluids with n-heptane and analyzed by using a reversed phase column and fluorescence detection of flunarizine. The detection limits were 1ng/ml of the plasma (serum) and 10ng/g of the brain and extraction recoveries were sufficiently high (89.5-100.2%). The method was applied to plasma samples from dogs after intravenous or oral administration (0.847mg/kg, flunarizine·22HCl 1mg/kg), and is possible to be applied to human serum samples and rat brain samples.View full abstractDownload PDF (528K) -
JIABI ZHU, KAZUNORI KATAYAMA, MASAWO KAKEMI, TAMOTSU KOIZUMI1986 Volume 106 Issue 3 Pages 221-227
Published: March 25, 1986
Released on J-STAGE: January 31, 2011
JOURNAL FREE ACCESSFour doses (5, 10, 20, 40mg) of furosemide were orally administered to 3 healthy male subjects. Urine samples were collected after predetermined time intervals and urinary excretions of the drug, Na+ and K+ were determined as well as urine volumes. Linear relationship was observed between increments ofcumulative Na++K+ excretion and urine volumes. Durations of diuretic response were about 3 h regardless of the dose administered, thereafter, Na++K+ excretions and urine volumes were below control levels. Three-hour cumulations of urinary Na++K+ excretion increments were linearly related to logarithm of the amount of furosemide administered.View full abstractDownload PDF (948K) -
MASATOSHI YAMAGUCHI, KEIKI TANNO1986 Volume 106 Issue 3 Pages 228-232
Published: March 25, 1986
Released on J-STAGE: January 31, 2011
JOURNAL FREE ACCESSA new methodology of a disintegration test for vaginal tablets was investigated. Samples from ten commercial vaginal tablets, five of which were effervescent and others noneffervescent types, were employed. A tablet was placed on the 9-mesh metallic net which was held horizontally at a designated position in distilled water at 37±0.5°C, and the guided plate was placed on the tablet. The guided plate moved downward smoothly in a cylinder as the tablet disintegrated. The movement was recorded by using the kymograph. The completion of the disintegration was defined at the time when the stable recording had started. The influence of the weight of the guided plate used on the disintegration time was investigated, and its optimum weight was found to be 4.0g. The desirable position of the metallic net was at a depth of 1.0mm by considering closer in vivo situation. With this method, the pharmaceutical properties of vaginal tablets were also observed. In comparison with other methods of disintegration test for vaginal tablets, satisfactory results for the proposed method were obtained. Thus, it can be concluded that this method provides a useful tool for the quality control test of vaginal tablets.View full abstractDownload PDF (3336K) -
SHINJI SHIBAMOTO, TAMIO NISHIMURA1986 Volume 106 Issue 3 Pages 233-239
Published: March 25, 1986
Released on J-STAGE: January 31, 2011
JOURNAL FREE ACCESSMethyl 3-[2-hydroxyimino-1-(4-chlorophenyl) ethylidene] dithiocarbazate was refluxed with potassium tert-butoxide in tert-butyl alcohol and the resulting potassium salt of 6-(4-chlorophenyl)-3-mercapto-1, 2, 4-triazine 4-oxide was S-methylated with CH3I. After reducing the 3-methylthio compound with triethyl phosphite, 6-(4-chlorophenyl)-3-methylthio-1, 2, 4-triazine was converted to the corresponding 3-hydrazino compound by the reaction with hydrazine. Then, 3-(substituted benzylidenehydrazino)-6-(4-chlorophenyl)-1, 2, 4-triazines, which were structurally similar to robenidine, were synthesized by reaction of the 3-hydrazino compound with benzaldehydes, and examined for their anticoccidial activity. 3-(4-Bromobenzylidenehydrazino)-6-(4-chlorophenyl)-1, 2, 4-triazine exhibited anticoccidial activity at a concentration of 50 ppm against E. tenella.View full abstractDownload PDF (808K) -
YASUYO OKADA, SHIZUYO HORIYAMA, KYOKO KOIZUMI1986 Volume 106 Issue 3 Pages 240-247
Published: March 25, 1986
Released on J-STAGE: January 31, 2011
JOURNAL FREE ACCESSCyclosophoraoses (CySs) are unbranched cyclic (1→2)-β-D-glucans (degree of polymerizations 17-40) produced by many strains of Agrobacterium and Rhizobium. CySs have larger cavity diameters and depths than cyclodextrins (CyDs), and are much more soluble in water than CyDs. Studies on inclusion complexes of non-steroidal anti-inflammatory agents (flurbiprofen, indomethacin, mefenamic acid, phenylbutazone) with CyS-A which is the CyS group member having the smallest molecular size were carried out by the solubility method, by using specimens prepared by four kinds of methods, I-IV. Solid inclusion complexes obtained by the method IV, in which CyS-A and the guest molecule were dissolved in aqueous ammonia and then the mixture was lyophilized, contained ammonia in the NH3/drug ratio of about 1 and it was suggested that CyS-A included nonsteroidal anti-inflammatory agent in the form of ammonium salt and stabilized this form. CyS-A does not exhibit hemolytic activity and depressed hemolysis by flurbiprofen and indomethacin.View full abstractDownload PDF (4597K) -
Mechanism of Antifungal Action of Propiolic Acid (β-Naphthyl) methyl EsterTOSHIO MAEDA, SADAYOSHI MATUI, MACHIKO HAYASHI, HIROSHI YAMAZOE, EIICH ...1986 Volume 106 Issue 3 Pages 248-256
Published: March 25, 1986
Released on J-STAGE: January 31, 2011
JOURNAL FREE ACCESSThe mechanism by which propiolic acid (β-naphthyl) methyl ester (PNE) caused an antifungal action on Candida albicans was studied. PNE inhibited the growth of C. albicans, and minimum inhibitory concentration and minimum fungicidal concentration were 6.25μg/ml and 12.5μg/ml, respectively. PNE at concentrations causing an antifungal action strongly inhibited the endogenous respiration, the exogenous respiration utilizing glucose, succinate, citrate and pyruvate, the uptakes of [3H] leucine and [3H] adenine into cells, the incorporation of [3H] leucine into trichloroacetic acid-precipitated fraction and the incorpporation of [3H] adenine into HClO4-precipitated fractions. However, the inhibitory actions of PNE were not observed in cell free system. During the incubation ofC. albicanswith PNE (12.5-25μg/ml), 20-30% of intracellular K+ was leaked, but leakages of protein and 260nm-absorbing materials were not observed. On the electromicroscopic observations, the surface of C. albicans was smooth and, 1 h after the treatment with PNE (12.5μg/ml), that was changed to be rough. After 24 h, big depressiens were found in almost fungi. These results suggcsted that PNE caused a damage in cell membrane ofC.albicansand that, as the results, the leakage of intracellular K+ and decrease in various metabolic functions of C.albicans occurred.View full abstractDownload PDF (3347K) -
SABURO SHIMABAYASHI, MASAHIRO KOJIMA, OSAMU KUSADA, MASAYUKI NAKAGAKI1986 Volume 106 Issue 3 Pages 257-259
Published: March 25, 1986
Released on J-STAGE: January 31, 2011
JOURNAL FREE ACCESSOrthophosphate ion (Pi) was detected in the precipitate formed by mixing K4P2O7 and CaCl2 in distilled water. The content of Pi in the precipitate increased with an increase in the amount of Ca2+ added, because diphosphate ion (PPi) was hydrolyzed to Pi in the presence of Ca2+. By means of X-ray powder diffractometry, CaK2P2O7·4H2O and Ca5K2-(P2O7)3·6H2O were found in the precipitate when molar ratio of mixing of CaCl2 to K4P2O7 was less than 2. On the other hand, when the molar ratio was higher than 2, the precipitate was amorphous immediately after mixing but diffraction peaks for hydroxyapatite (HAP; Ca10 (PO4)6(OH)2) were observed after aging for 2 weeks at 30°C. The degree of crystallinity of HAP and that of hydrolysis of PPi to Pi, however, were lower than those of the precipitate obtained by mixing the reagents in alkaline solution (KOH or NH4OH).View full abstractDownload PDF (498K) -
MICHITARO FUJIMOTO, MASANORI KATSURADA1986 Volume 106 Issue 3 Pages 260-264
Published: March 25, 1986
Released on J-STAGE: January 31, 2011
JOURNAL FREE ACCESSThe reaction of 4 (5)-bromo-5 (4)-methylimidazole (1) with methanethiol or benzenethiol in N, N-dimethylformamide in the presence of sodium hydride was found to give not only the corresponding substituted products (2a, b) but also a debromo compound, 4 (5)-methylimidazole (3). By the similar reaction of 3-bromoquinoline (4), 4-bromoisoquinoline (6) and 3-bromopyridine (8) with various kinds of thiol, only the corresponding substituted products (5a-d, 7a-d, 9a, b) were obtained in good yield, respectively, and the formation of debromo compounds such as those described above was not detected.View full abstractDownload PDF (503K) -
Separation of Myoglobin from Different Species (Sperm Whale, Horse) by Reversed Phase High Performance Liquid ChromatographySUSUMU IWAKIRI, NAOKI ASAKAWA, TAKESHI MIYAKAWA, YASUO MIYAKE1986 Volume 106 Issue 3 Pages 265-267
Published: March 25, 1986
Released on J-STAGE: January 31, 2011
JOURNAL FREE ACCESSSimultaneous and efficient separation of sperm whale and horse myoglobins were examined by use of reversed-phase high performance liquid chromatographic (RP-HPLC) method for insulins described in our previous reports. The separation of both myoglobins was reported here under isocratic elution system on a column of Nucleosil CN with a mixture of acetonitrile and phosphate buffer (pH 3.0) containing sodium perchlorate as mobile phase.View full abstractDownload PDF (370K)
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