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Volume 9, Issue 10
Displaying 1-13 of 13 articles from this issue
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Wataru Nagata, Tadao Terasawa1961 Volume 9 Issue 10 Pages 745-755
Published: October 25, 1961
Released on J-STAGE: March 31, 2008
JOURNAL FREE ACCESSPersaureoxydation von 6-Methoxy-3, 4-dihydronaphthalin (I) verlief unter einer abnormalen Aufspaltung des intermediar entstandene Epoxides und ergab ein Gemisch von cis- und trans-Monoacyldiolen, bevorzugt mit dem ersteren. Das Entstehen von cis-1-Acetoxy-2-benzoyloxy-6-methoxy-1, 2, 3, 4-tetrahydronaphthalin (IIIa) bei der Oxydation mit Benzopersaure und bei der nachtraglichen Acetylierung ist durch eine intramolekulare Umesterung des zuerst entstehenden cis-1-Monobenzoates (XIVa) (R=Phenyl) erklarbar. Eine derartige Wechselwirkung des cis-1, 2-Diolderivates wurde auch beim cis-Diacetat (IIa) beobachtet. Trans-Diol (VIIIb) ergab durch Einwirkung von Aceton oder p-Nitrobenzaldehyd cis-Dioxoran-Verbindungen (IX oder X). Diese abnormalen Ergebnisse konnen durch Annahme der auβerst stabilen C1-Carboniumionen und der Wechselwirkung der cis stehenden benachtbaren Substituenten sehr gut erklart werden.View full abstractDownload PDF (1420K) -
Wataru Nagata, Shoichi Hirai, Tadao Terasawa, Ikuo Kikkawa, Kenichi Ta ...1961 Volume 9 Issue 10 Pages 756-768
Published: October 25, 1961
Released on J-STAGE: March 31, 2008
JOURNAL FREE ACCESSAusgehend von 6-Methoxy-3, 4-dihydronaphthalin-2(1H)-on (III) wurden durch Anwendung der Robinson'schen Methode die tricyclischen Ketone (IVa), (VIIIa) und (VIIIb), sowie das tetracyclische Keton (XXI) in guter Ausbeute erhalten und die Strukturen der Nebensowie Zwischen-Produkte wurden ermittelt.View full abstractDownload PDF (1718K) -
Wataru Nagata, Shoichi Hirai, Tadao Terasawa, Kenichi Takeda1961 Volume 9 Issue 10 Pages 769-783
Published: October 25, 1961
Released on J-STAGE: March 31, 2008
JOURNAL FREE ACCESSDas zur Totalsynthese der Steroide sehr wichtige Zwischenprodukt, namlich rac-3β-Hydroxy-D-homo-18-nor-5α-androst-13(17a)-en-17-on (Va) wurde aus tetracyclischem Keton (III) auf einer Stufe durch Lithium-Alkohol-Ammoniak-Reduktion nach der Wilds-Nelson'schen Art hergestellt. Es wurde noch festgestellt, daβ das dabei als Nebenprodukt entstandene Produkt ein an C8 und C14 epimeres Raumisomer (VIa) darstellt. Dihydro-sowie Tetrahydroverbindungen mit dem Anisolgerust, die sich alle als Zwischen-produkte zum (Va) sowie (VIa) bei dieser Reduktion ansehen lieβen, wurden hergestellt und deren Strukturen sowie raumliche Anordnungen wurden ermittelt. Ferner wurde der Mechanismus betreffs der Metall-Ammoniak-Alkohol-Reduktion von Styroltypen-Verbindungen diskutiert.View full abstractDownload PDF (1749K) -
Wataru Nagata, Tadao Terasawa, Tsutomu Aoki, Kenichi Takeda1961 Volume 9 Issue 10 Pages 783-795
Published: October 25, 1961
Released on J-STAGE: March 31, 2008
JOURNAL FREE ACCESSDurch Einwirkung von Kaliumcyanid und anschlieβende Acetylierung lieβ sich rac-3β-Hydroxy-D-homo-18-nor-5α-androst-13 (17a)-en-17-on (I) unter der 1, 4-Additionsreaktion des Cyanidions und nachfolgender Verseifung glatt in die epimere Brucken-Verbindung, namlich (13∼17) β-sowie (13∼17) α-Laktamol (IV), (V) und deren Acetate (VI) und (VII) verwandeln. Ferner wurden durch Abanderung der nachtraglichen Reaktionsfolgen, z. B. Alkylierung und Acetylierung oder Oxydierung, eine Reihe von beim C13 epimeren C17-Alkoxylaktamolen, z. B. (VIII), (IX), (X), (XI), (XX) und (XXI), synthetisiert. Die 13-Cyanverbindungen, wie (XV), (XVI) und (XVII), konnten erst durch kurze Einwirkung von Kaliumcyanid auf (III) oder durch Verwendung einer begrenzten Menge von Kaliumcyanid an (I)-Acetat (II) hergestellt werden. Die raumlichen Strukturen aller hierbei erhaltenen Verbindungen wurden ermittelt. Die hier eingefuhrten Reaktionsfolgen stellen eine neue Method fur die Einfuhrung der angularen C-Substituente dar und lieferten einen Anhaltspunkt zur Totalsynthese der normalen sowie 18-funktionierten Steroide.View full abstractDownload PDF (1804K) -
Yoshinobu Nakai1961 Volume 9 Issue 10 Pages 796-800
Published: October 25, 1961
Released on J-STAGE: March 31, 2008
JOURNAL FREE ACCESSThe characteristic values of tablet disintegration by thermal analysis were considered theoretically and their physical meaning was examined. The graphic surface area, α, enclosed by the curve of surface area in solution and time axis, was calculated for a powder system and it was proved that the value of α was constant for the same substance and experimental conditions. Moreover it was proved theoretically and experimentally that the graphic surface area of the same weight of powder was constant in total amount when the powder was divided and measured. This result of a powder could be applied to a tablet and the integral snrface area of a tablet was constant for the same weight. The experimental results agreed with this theory, and it was proved that the meaning of S2×t3 was similar to the integral surface area. The mean volume surface diameter is related to the largest particle size evaluated in tablet disintegration. From these theoretical considerations, the physical meaning of the value of U. S. P. method was discussed and elucidated.View full abstractDownload PDF (518K) -
Yasuo Makisumi1961 Volume 9 Issue 10 Pages 801-808
Published: October 25, 1961
Released on J-STAGE: March 31, 2008
JOURNAL FREE ACCESSThe products of the condensation of 5-amino-s-triazole (I) with ethyl malonate, ethyl cyanoacetate, and methyl ethoxycarbonyldithioacetate were proved to be respectively 5, 7-dihydroxy-, 5-hydroxy-7-amino-, and 5-hydroxy-7-mercapto-s-triazolo [2, 3-a] pyriminines (II, III, and IV). (II) was converted into the 5, 7-dichloro derivative (VI), and the reactivity of the two halogens in (VI) towards the usual nucleophilic reagents was examined. (IV) was also transformed into the 5-chloro-7-methylthio derivative (XXI), which was converted into 5-substituted 7-methylthio derivatives by nucleophilic substitution. Ultraviolet absorption spectra of 5-substituted and 7-substituted s-triazolo [2, 3-a] pyrimidines were compared.View full abstractDownload PDF (976K) -
Yasuo Makisumi1961 Volume 9 Issue 10 Pages 808-814
Published: October 25, 1961
Released on J-STAGE: March 31, 2008
JOURNAL FREE ACCESSHalogenation of s-triazolo [2, 3-a] pyrimidine and its 5-methyl derivative with chlorine or bromine gave the corresponding 6-halo derivative (IIIa, IIIb, IVa, and IVb), but in the case of 5-hydroxy-7-amino-and 5, 7-dihydroxy-s-triazolo [2. 3-a] pyrimidines, reaction of bromine gave 6-bromo derivatives (VIIb and VIIIb) while that of chlorine gave 5-dichloro-acetamido-s-triazole (IX) instead of 6-chloro derivatives (VIIa and VIIIa). 2-Halo-1, 3-dicarbonyl compounds were condensed with 5-amino-s-triazole (X) into 6-chloro-s-triazolo-[2, 3-a] pyrimidines (VIa, VIIa, and VIIIa), but 6-bromo derivatives were not obtained due to resinification. Ultraviolet spectra of 19 kinds of 6-halo-s-triazolo [2, 3-a] pyrimidines were measured and compared with those of the corresponding original compounds.View full abstractDownload PDF (773K) -
Synthesis of Potential Anticancer Agents. VI. Reactivity of 6-Bromo-s-triazolo [2, 3-a] pyrimidines.Yasuo Makisumi1961 Volume 9 Issue 10 Pages 814-817
Published: October 25, 1961
Released on J-STAGE: March 31, 2008
JOURNAL FREE ACCESS5-Hydroxy-6-bromo-7-amino- and 5, 7-dihydroxy-6-bromo-s-triazolo [2, 3-a] pyrimidines (III and IV) reacted with piperidine or morpholine to form the corresponding 6-piperidino-(V and VII) or morpholino-(VI and VIII) derivatives. Reaction of (IV) with thiourea gave the 6-amidinothio derivative (IX), which was converted into disulfide compound (X) by the action of alkali. Reaction of (III) with thiourea gave the 5-hydroxy-7-amino derivative (XII) and this reaction in alkaline medium gave the sulfide compound (XIII).View full abstractDownload PDF (526K) -
Tomishige Mizoguchi1961 Volume 9 Issue 10 Pages 818-826
Published: October 25, 1961
Released on J-STAGE: March 31, 2008
JOURNAL FREE ACCESSA new synthesis of rac-nicotine was described. For this end the removal of the benzylidene group of 2-substituted 3-benzylidene-1-pyrroline prepared by Sugasawa and Ushioda was first examined. For the best effect, the starting materials ((I) : 2-methyl ; (IXa) : 2-phenyl) were reduced by sodium borohydride and the reduction products were acylated to yield ((IIIa) : 1-acetyl-2-methyl ; (IIIb) : 1-benzoyl-2-methyl ; (XIIa) : 1-benzoyl-2-phenyl). These were cleaved via the corresponding ozonides to yield 3-pyrrolidinones, which were characterized appropriately. This method was successfully extended to 2-(3-pyridyl)-3-benzylidene-1-pyrroline to afford 1-benzoyl-2-(3-pyridyl)-3-pyrrolidinone, whose tosylhydrazone was converted into 1-benzoyl-2-(3-pyridyl)-3-pyrroline according to the method of Bamford and Stevens. The latter was reduced catalytically to rac-nornicotine, from which rac-nicotine was obtained smoothly by Eschweiler-Clark's method.View full abstractDownload PDF (1157K) -
Toshio Miyazaki1961 Volume 9 Issue 10 Pages 826-829
Published: October 25, 1961
Released on J-STAGE: March 31, 2008
JOURNAL FREE ACCESSCapsular polysaccharide of the Cryptococcus neoformans was found to be a xyloglucu-ronomannan, which consisted of D-glucuronic acid, D-xylose, and D-mannose (in 1 : 1 : 3 ratio), and its molecular weight was about 6600 by the Akiya-Barger's method and from results of end-group assay. D-Xylose and a part of D-glucuronic acid in this polysaccharide were liberated more easily than D-mannose.View full abstractDownload PDF (566K) -
Toshio Miyazaki1961 Volume 9 Issue 10 Pages 829-833
Published: October 25, 1961
Released on J-STAGE: March 31, 2008
JOURNAL FREE ACCESSThe chemical structure of the capsular polysaccharide from Cryptococcus neoformans was further investigated by periodate oxidation and methylation. Periodate oxidation of the polysaccharide produced formic acid and formaldehyde, and the xylose and glucuronic acid were attacked, but a part of mannose was resistant. Hydrolysis of the methylated polysaccharide gave 2, 3, 4-tri-O-methyl-D-xylose, 2, 3, 6-tri-O-methyl-D-monnose, 2, 3, 4-tri-O-methyl-D-glucuronic acid, and 3, 6-di-O-methyl-D-mannose in 1 : 1 : 1 : 2 ratio. From these results, the chemical structure of this polysaccharide was proposed.View full abstractDownload PDF (605K) -
Hiroshi Watanabe, Shigeru Kuwata, Sugao Koyama1961 Volume 9 Issue 10 Pages 834-835
Published: October 25, 1961
Released on J-STAGE: March 31, 2008
JOURNAL FREE ACCESSDownload PDF (349K) -
Kyosuke Tsuda, Kiyoshi Sakai, Nobuo Ikekawa1961 Volume 9 Issue 10 Pages 835-836
Published: October 25, 1961
Released on J-STAGE: March 31, 2008
JOURNAL FREE ACCESSDownload PDF (337K)
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