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Volume 70, Issue 11
Displaying 1-19 of 19 articles from this issue
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Tetsuro Matsumoto1950 Volume 70 Issue 11 Pages 595-600
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSIsolation of aliphatic primary, secondary and tertiary amines, including ammonia, by partial neutralization and steam distillation was carried out, with examination of the purity of each amine distillate. These amines can be classified into strongly basic group (primary and secondary amines) and the weakly basic group (tertiary amine and ammonia). Partial neutralization allows separation of amines from a mixture of the two groups, but does not make it possible to separate the amines of one group into each component. Quantitative estimation of amines were carried out by the van Slyke method for primary amines with ammonia, the tertiary amines after treatment with nitrous acid, secondary amines, by the difference with total basicity, and ammonia, by Na3Co(NO2)6 as described in the previous report. From this result, a systematic method of isolation of aliphatic amine hydrochloride was completed.
Extraction of the hydrochloride of amines by chloroform results in solution of the secondary and tertiary amine hydrochlorides with primary amine hydrochloride and ammonium chloride remaining in the solution. Since each of these groups are combinations of strongly and weakly basic compounds, the respective components can be isolated by partial neutralization.View full abstractDownload PDF (1078K) -
Synthesis of dl-Tuberculostearic Acid. (2)Mitizo Asano, Jisaku Ota1950 Volume 70 Issue 11 Pages 601-605
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSIn order to find the best method of synthesizing tuberculostearic acid, a branched-chain fatty acid contained in the lipoid of tubercle bacilli, a mixture of the lead salts of α-methyloctylacetic acid and ethyl hydrogen azelate was dry-distilled to obtain ketonic acid but the reaction was unsuccessful. Attempt was then made for the Kolbe's electrolysis of potassium α-methyloctylacetate and potassium salt of ethyl hydrogen sebacate by which a racemic acid was obtained. Acid amide of this dl-tuberculostearic acid melted at 80-81.5°.View full abstractDownload PDF (988K) -
Jun Mizuguchi1950 Volume 70 Issue 11 Pages 605-610
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSAn attempt was made to improve the electrolytic method whereby calcium gluconate could be prepared in a minimum period. In order to make it possible to allow electrolysis by the maximum current concentration, cooling system must be sufficiently performing. However, these cooling systems were of glass or porcelain up to the present which did not give sufficient cooling.
In the present experiment, Pb, Cu, Ni, and Ag metals were used as the cooler wall which was utilized as the cathode in order to avoid rusting of these metals. Test electrolysis with various compositions of electrolytic media showed that those metals used, especially Ag, in contact with the media were hardly corroded. It was also shown that no difference in electric efficiency, yield of the product or its quality existed between these experimental products and those obtained with the usual carbon cathode. These have provided good data for the construction of commercial electrolytic cell.View full abstractDownload PDF (1014K) -
Jun Mizuguchi1950 Volume 70 Issue 11 Pages 610-613
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSA metal electrolytic cell of closed, forced-circulation type, was designed, constructed and experimentally run, with copper as the metallic material. As a result, it was found that at 15l. capacity, using 250A and 11.5V, the cooling was sufficient, and forced circulation of the electrolyte solution showed sufficient stirring effect.
It is assumed that, by the use of this electrolytic cell, ordinary electrolysis will be completed in 4.5-7 hours by electric current of 250-150A. The diagram gives details of the cell, and the results of experimental runs are given in the table.View full abstractDownload PDF (811K) -
Jun Mizuguchi1950 Volume 70 Issue 11 Pages 613-616
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSIn continuation of the experiments reported in I and II, experimental manufacture was carried out of calcium gluconate from glucose obtained electrolytically by the use of the closed, forced-circulation type metallic electrolytic cell. As a result, it has been established that the time of electrolysis was completed within a few hours, as expected. The use of easily corrosive copper as the cathode and a cooling wall, showed the loss of the electrolytic cell to be negligible. It was also proved, by obtaining J. P. quality calcium gluconate after two recrystallizations, that Cu ion occluded in the preparation is also negligible. Satisfactory results were also obtained on mechanical problems, such as stirring, cooling, etc., and the loss of bromine was also lowered far below that in the open-type electrolytic cell.
It could, therefore, be concluded that this new method using experimental electrolytic cell can be used in practical application. In the event of the industrialization of this method to continuous production, the inside walls of the electrolytic cell could be lined or plated with silver, and, if the recovery of bromine from waste gas can be carried out, it would offer an advantageous method over the classic method.View full abstractDownload PDF (702K) -
Tsutomu Momose, Tatsuo Schoji1950 Volume 70 Issue 11 Pages 616-618
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSp-Aminomethylphenyl methyl sulfone was prepared from p-formylamino- or p-phthalimino-methylphenyl sulfochloride which was first reduced to sulfinic acid, treated by methyl iodide in alkaline state to sulfone, and subsequently saponified to remove the formyl or phthalyl group. This method gives the objective compound in a better yield than that starting from p-acetylaminomethylphenyl sulfochloride.
On the other hand, p-aminomethylphenyl alkyl sulfones were prepared from p-methylphenyl alkyl sulfones which were oxidized to p-aldehydephenyl alkyl sulfones, the oximes of which were reduced to obtain the objective compounds.View full abstractDownload PDF (481K) -
Synthesis of 3, 4-(m, m′-Dimethyl-p, p′-dipropoxydiphenyl)-n-hexaneShobun Tanabe, Sadao Onishi1950 Volume 70 Issue 11 Pages 618-621
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSHexene (2)-ol (4), was reacted resp. with anisol and o-cresylmethyl ether with conc. H2SO4 as a condensing agent, and 3, 4-(p, p′-dimethoxydiphenyl)-n-hexane and 3, 4-(m, m′-dimethyl-p, p′-dimethoxydiphenyl)-n-hexane, respectively, were obtained.
The structures of these compounds were proved by the direct comparison with the standard products obtained by other synthetic method, and also from analytical values. Demethylation of 3, 4-(m, m′-dimethyl-p, p′-dimethoxydiphenyl)-n-hexane gave 3, 4-(m, m′-dimethyl-p, p′-dihydroxydiphenyl)-n-hexane from which dipropionate and dibenzoate of the subject compound were obtained. The comparison of the synthesized 3, 4-(m, m′-dimethyl-p, p′-dihydroxydiphenyl)-n-hexane with the data in literature showed a difference of 21-22° in the melting point. Reason for this difference is at present unknown. The synthetic compounds obtained in the present experiment will be put to animal test as to the presence of sexual excitation.View full abstractDownload PDF (621K) -
Syntheses of Fatty Acids with Phenyl Group in α- and β-PositionsMitizo Asano, Hiroko Motomatsu, Osamu Tamemasa1950 Volume 70 Issue 11 Pages 622-625
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSIn order to examine the relationship between chemical structure and antibacterial power of branched-chain fatty acids, fatty acids possessing benzene ring in the α- and β-positions were synthesized. The compounds synthesized were: R-CH(C6H5)-COOH type in which R were CH3, C2H5, n-C4H9, n-C8H17, n-C10H21, n-C12H25, n-C13H27, and n-C14H29; R-CH(C6H5)-CH2-COOH type in which R were CH3, n-C3H7, n-C7H15, n-C9H19, n-C11H23, and n-C15H31. The compounds of the former type were obtained by the alkylation of phenylmalonic ester with alkyl halides, and the latter by the condensation of phenylalkylmethane chloride with malonic ester with subsequent saponification and decarboxylation.View full abstractDownload PDF (741K) -
Zyuniti Hase1950 Volume 70 Issue 11 Pages 625-629
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSAs a method for the synthesis of polyhydroxynaphthoquinones, 2-ethyl-3, 6, 7, 8-tetrahydroxy-1, 4-naphthoquinone was synthesized by the following course: Starting with ethyl 3, 4, 5-trimethoxybenzoylacetate, it passed through diethyl α-ethyl-β-3, 4, 5-trimethoxybenzoylsuccinate, α-ethyl-β-3, 4, 5-trimethoxybenzoylpropionic acid, α-ethyl-γ-3, 4, 5-trimethoxyphenylbutyric acid, 2-ethyl-6, 7, 8-trimethoxytetralone-(1), 2-ethyl-6, 7, 8-trimethoxynaphthol-(1), 2-ethyl-6, 7, 8-trimethoxy-1, 4-naphthoquinone and its 2, 3-oxide, and 2-ethyl-3-hydroxy-6, 7, 8-trimethoxy-1, 4-naphthoquinone, and finally to 2-ethyl-3, 6, 7, 8-tetrahydroxy-1, 4-naphthoquinone. Coloration of hydroxynaphthoquinones to bicarbonate, sodium hydroxide and lead acetate was compared.View full abstractDownload PDF (899K) -
Immune Test with ButhotoxinTenmin Kaku, Yoshitoshi Kase, Tadayuki Sakuma1950 Volume 70 Issue 11 Pages 629-632
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSIn order to prepare rabbit serum immune to buthotoxin, crude buthotoxin sulfate was injected subcutaneously into rabbits, later intravenously, in small portions. The completion of immunization on the 19th day (total dose of the venom used, 11320γ) was tested with mice and the immunization was recognized to be 1.33 times of m.l.d. of mice.
It was confirmed that the sera of cats and of nonpoisonous snake (Elaphe climacophora Boie) can detoxicate and neutralize buthotoxin to a slight degree.
The crystalline picrate of a component reported in the preceeding paper as being chemically unknown was identified as hydroxylamine picrate.View full abstractDownload PDF (690K) -
A Contribution to the Biochemical Breakdown of Fatty Acids in Natural SeriesTamio Yamakawa1950 Volume 70 Issue 11 Pages 633-637
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSIn order to understand the oxidation cleavage of fatty acids in which the number of carbon atoms is in the range of those appearing in nature, 2-propylmyristic acid was given to rabbits and 2-propyladipic acid was recovered from their urine. Comparing this result with the works carried out by earlier researchers, a hypothesis of ζ-oxidation was proposed. However, when the rabbits were given 2-propyltridecanoic acid, from their urine was recovered a mixture of acids in 70-30 gravimetric proportions of 2-propylglutaric and 2-propylpimelic acids by which the possibility of ζ-oxidation was completely lost. It was further confirmed that branched-chain fatty acids possessing 16-17 C-atoms underwent ω-oxidation at first, then β-oxidation, finally liberating the two C-atom fragments from the end.View full abstractDownload PDF (930K) -
Syntheses of p-Hydroxybenzene-sulfonamide Derivatives. (2)Taizo Matsukawa, Buhachiro Ohta, Yoshiko Morita1950 Volume 70 Issue 11 Pages 638-640
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSEight kinds of 2-(p-hydroxybenzenesulfonamino)-pyrimidine derivatives were obtained by fusion of p-hydroxybenzene-sulfonamide and 2-alkylmercaptopyrimidines.View full abstractDownload PDF (574K) -
A Method of Estimation of 6-α-Glucosylglucose and Gentiobiose formed from GlucoseTsukinaka Yamana1950 Volume 70 Issue 11 Pages 641-643
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSGentiobiose was quantitatively determined by the increase of its reductive power by the hydrolysis of gentiobiose by Takadiastase. Gentiobiose was determined in a similar manner in the non-fermenting sugars formed from glucose. By the use of Somogyi's microanalytical method for sugar determination, only about 2mg. of sample is necessary. Following observations were also obtained:
1) The reductive power of gentiobiose against Somogyi's reagent corresponds to 0.542 of glucose.
2) The hydrolysis rate of commercial Takadiastase against gentiobiose is about 10 times faster than the hydrolysis rate of the standard emulsin prepared from almond seeds by the Helferich method (omitting purification by silver oxide).View full abstractDownload PDF (648K) -
Takashi Saeki1950 Volume 70 Issue 11 Pages 644-653
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSTitration tank which do not use the ordinary calomel electrode used in ordinary potential titration, and a voltage amplifier of high sensitivity were experimentally manufactured used.View full abstractDownload PDF (1454K) -
Takashi Saeki1950 Volume 70 Issue 11 Pages 653-660
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSAn automatic stopping device, a pusher-type burette, and a spark-type automatic recorder, were experimentally manufactured and used for the automatization of potential titration apparatus.View full abstractDownload PDF (1085K) -
Takashi Saeki1950 Volume 70 Issue 11 Pages 660-668
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSQuantitative determination of sulfonamide by diazotisation, stipulated in U.S.P. XII, was carried out by potential titration and an excellent result was obtained. As a result, this titration can be applied to purity determination of chemicals belonging to the aromatic amine series.View full abstractDownload PDF (1290K) -
Harutada Negoro1950 Volume 70 Issue 11 Pages 669-670
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSDownload PDF (349K) -
Michihiro Hirai, Ryoichi Hayatsu1950 Volume 70 Issue 11 Pages 670-671
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSDownload PDF (379K) -
[in Japanese], [in Japanese]1950 Volume 70 Issue 11 Pages 672
Published: November 25, 1950
Released on J-STAGE: February 19, 2010
JOURNAL FREE ACCESSDownload PDF (209K)
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