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Volume 25, Issue 2
Displaying 1-10 of 10 articles from this issue
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Yoshixo OGATA1967 Volume 25 Issue 2 Pages 101-115
Published: February 01, 1967
Released on J-STAGE: June 28, 2010
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Masaru HASEGAWA1967 Volume 25 Issue 2 Pages 116-126
Published: February 01, 1967
Released on J-STAGE: March 01, 2011
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Syntheses of gem-dimethylalkylenediamines and their polyureasKosuke YAMAMOTO, Goro KIMURA1967 Volume 25 Issue 2 Pages 127-136
Published: February 01, 1967
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSgem-Dimethylalkylenediamines, H2N(CH2)m-CH3-C-CH3-(CH2)nNH2 (m, n: 1-5), were synthesized and treated with urea to obtain polyureas of symmetric side chain structures. Upon treatment with hydrogen chloride, isoprene and methallyl chloride were converted into the corresponding dichlorides. Since one of the chlorine atoms of the dichloride is tertiary, one or two ethylene molecules can be introduced between the carbon and chlorine atoms, giving gem-dimethyalkylenedichloride. With subsequent cyanation followed by hydrogenation, desired gem-dimethylalkylenediamines were obtained. All the polyureas so obtained were transparent and could be spun into fibers. Their melting points and specific gravities were considerably low as compared with that of linear alkylenediamine polyureas, as follows:View full abstractDownload PDF (1263K) -
Catalytic Dealcohalation of Acetaldehyde Diethylaceatal over CaSo4 CatalystMlchitoshi KITABATAKE, Sakahiko OWARI, Koichi KUNO1967 Volume 25 Issue 2 Pages 137-143
Published: February 01, 1967
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSCatalytic dealcoholation of acetaldehyde diethylacetal over calcium sulfate catalyst has been studied in a flow system. Data for the conversion of acetal versus W/F curves were obtained at three temperatures, 174, 188, and 200°C. It seems reasonable to assume that the reaction is reversible. Equilibrium constants, Kp, were determined and the following equation derived. log Kp=-3.84×103/T+8.243 A rate equation was established and the apparent activation energy was calculated to be 21 Kcal/mol. Effects of ethyl vinyl ether, ethanol, and water added to the acetal were also examined.View full abstractDownload PDF (678K) -
Ichiro HASHIMOTO, Minoru TASHIRO1967 Volume 25 Issue 2 Pages 144-149
Published: February 01, 1967
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSXylylene diamines were smoothly and selectively hydrogenated into the corresponding bis(aminomethyl)cyclohexanes in the presence of newly modified ruthenium catalysts. They were prepared by heating sodium ruthenate supported on active carbon under carbon dioxide atmosphere. Commercial ruthenium catalysts were not active enough to complete the hydrogenation in contrast with their full activity for aniline. The hydrogenation reaction of m-xylylenediamine is zero order in diamine concentration and first order in hydrogen pressure. Small quantities of m-methylbenzylamine, 1-aminomethyl-3-methylcyclohexane, and m-xylene were formed as byproducts presumably from the starting diamine through hydrogenolysis. Apparent activation energy for the formaton of 1, 3-bis(aminomethyl)cyclohexane was found to be 8.6 Kcal/mol. Though m-xylylenediamine gave predominantly cis-bis(aminomethyl)cyclohexane, almost 1 to 1 mixture of cis-and trans-isomers was obtained from p-xylylenediamine.View full abstractDownload PDF (775K) -
Yasuhiko DOZEN, Shizu FUJISHIMA1967 Volume 25 Issue 2 Pages 150-154
Published: February 01, 1967
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSPotassium permanganate oxidation of alkyl benzoic acids and pseudocumene has been carried out in an aqueous alkaline solution. 2, 4-and 2, 5-Dimethylbenzoic acids gave 2-methylterephthalic acid and 4-methylisophthalic acid, respectively, as an intermediate in the preparation of trimellitic acid. In the oxidation of 3, 4- dimethylbenzoic acid and competitive oxidation of isomeric toluic acids, the relative reactivity of the methyl groups has been established, as follows : para>reta>ortho. By partial oxidation of mesitoic acid, 2, 6-dimethylterephthalic acid was obtained as main product. In the case of pseudocumene, 2, 4-and 3, 4-dimethylbenzoic, 2-metylterephthalic, and 4-methylisophthalic acids were produced as intermediate products. Their formations were explained by the difference in relative reactivities of the methyl groups.View full abstractDownload PDF (688K) -
Reaction of Potassium Benzoate in the Presence of Potassium Carbonate and Potassium Cyanate.Yasuhiko DOZEN, Shizu FUJISHIMA1967 Volume 25 Issue 2 Pages 155-160
Published: February 01, 1967
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSReactions of potassium benzoate in the presence of potassium carbonate and cyanate have been studied under various conditions. The acids formed were analyzed by vapor phase chromatography after esterification with diazomethane. Maximum yield of terephthalic acid (ca. 60%) was obtained at 380-405°C in 3 hrs and longer heating failed to improve the yield. Effects of the pressure of carbon dioxide and of the molar ratio of potassium carbonate to potassium benzoate were evident. The anion moieties of cadmium compounds did not affect the composition of the products, and the yield of terephthalic acid and the conversion of potassium benzoate were rather reduced in the presence of a large amount of potassium cyanate. In an initial stage of this reaction, considerable amounts of phthalic, isophthalic, and benzene tricarboxylic acids were formed together with terephthalic acid. The direct carboxylation of potassium benzoate with potassium carbonate in potassium cyanate was indicated from the fact that the yield of terephthalic acid was higher than that expected from the disproportionation reaction. On the other hand, in the reaction of sodium benzoate in the presence of sodium cyanate and sodium carbonate, the effect of sodium cyanate could not be demonstrated.In an initial stage of this reaction, sodium benzoate gave only sodium phthalate.View full abstractDownload PDF (898K) -
Synthesis of N-(2-Acetoxy-3(or 4, 5)-methylbenzoyl)melamines and their Use for the Synthesis of DyesHidehiko KITAJIMA, Yoshibumi OSHIMA, Yoshinari KUROKAWA, Toyoshi YAMAD ...1967 Volume 25 Issue 2 Pages 161-166
Published: February 01, 1967
Released on J-STAGE: March 01, 2011
JOURNAL FREE ACCESSAcetyl-o (or m, p)-cresotic anhydrides were synthesized in good yield from the corresponding acetylcresotic acids and thionyl chloride in the presence of pyridine. Mixtures of melamine and acetylcresotic anhydrides dissolved in dioxane were heated to reflux to obtain N-(2-acetoxy-x-methylbenzoyl)melamines (x: 3, (1) ; 4, (4); 5, (7)). The corresponding N, N'-diacylmelamines were formed as by-products as identified in the forms of hydroxy derivatives (x: 3, (3); 4, (6) ; 5, (9)). Upon hydrolysis with 10% aqueous pyridine, (1), (4), and (7) gave the corresponding hydroxy derivatives ((2), (5), and (8)). Acetylcresotic anhydrides and the melamine derivatives ((1)-(9)) are new compounds not found in the literatures. Azo dyes were synthesized using (2), (3), (5), and (8) as coupling components, and the dyeingabilities of their methylol compounds for cotton and rayon investigated.View full abstractDownload PDF (884K) -
Goro KIMURA1967 Volume 25 Issue 2 Pages 167-179
Published: February 01, 1967
Released on J-STAGE: July 05, 2011
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Keiichi SUZUKI1967 Volume 25 Issue 2 Pages 180-183
Published: February 01, 1967
Released on J-STAGE: June 28, 2010
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