有機合成化学協会誌
Online ISSN : 1883-6526
Print ISSN : 0037-9980
ISSN-L : 0037-9980
20 巻, 2 号
選択された号の論文の11件中1~11を表示しています
  • 村上 謙吉
    1962 年 20 巻 2 号 p. 103-126
    発行日: 1962/02/01
    公開日: 2011/03/01
    ジャーナル フリー
  • 団野 晧文
    1962 年 20 巻 2 号 p. 127-142
    発行日: 1962/02/01
    公開日: 2011/03/01
    ジャーナル フリー
  • 線型キナクリドンの合成
    橋爪 清
    1962 年 20 巻 2 号 p. 143-145
    発行日: 1962/02/01
    公開日: 2011/03/01
    ジャーナル フリー
    As a method for synthesis of linear type quinacridone (1), a valuable organic pigment of red coloration is made through 2, 5-dihaloterephthalic acid (8) and 2, 5-dianilinoterephthalic acid (2). Heating of 2, 5-dibromoterephthalic acid and aniline in dimethylf ormamide in the presence of cuprous chloride and copper powder for 8 hours at 153$deg;c yielded 50-70% of theory of (2). Heating of (2) in phosphorus oxychloride and anhydrous aluminum chloride for 6 hours at 100-110°c yielded 87% of theory of (1).
  • α-クロルアクリル酸エステルの重合体の製造
    平井 浩
    1962 年 20 巻 2 号 p. 146-149
    発行日: 1962/02/01
    公開日: 2010/06/28
    ジャーナル フリー
    Foregoing experiments indicated that heretofore considered cause of coloration merely by the effect of peroxide is errorneous but the cause is supporsed to be due to oxalyl halide derived from the peroxide as shown by experimental facts. It was found unnecessary to exclude air during the polymerization and storage by addition of a suitable substance which is effective for inactivation of oxalyl halide. However, the addition of above a certain amount is found to be harmful in keeping the quality of polymerized methyl α-chloracrylate. It was found that the polymerization for 18-24 hours at 110-30°c gave good plastic material having high hardness. B.P.O., succinyl peroxide and peracetic acid as the catalysts, which are generally used for polymerization of vinyl compounds, are found to be effective. Since the defect of coloration of methyl α-chloracrylate for practical use was improved by an addition of suitable additive agent and ite superior hardness, mechanical strength, and heat-resistance than usual methyl methacrylate polymer, the future development of this type of plastic is much anticipated. As for substance to be added, lower monohydric alcohols, such as methanol, isopropanol and butanol, are effective additive agents and these are obtainable at low cost. By addition of additive agent, a complete exclusion of air was unnecessay and this brought a considerable improvement in the handling of the monomer in chemical and industrial operations.
  • 斎藤 鐘次郎, 立花 輝一, 大道 弘昭
    1962 年 20 巻 2 号 p. 150-157
    発行日: 1962/02/01
    公開日: 2011/07/05
    ジャーナル フリー
    6-Methyl-6 (or 5)-hepten-2-one was synthesized from the addition compounds which were prepared from 4-methyl-l-penten-3-ol acetate or 2-methyl-4-penten-2-ol acetate and acetaldehyde by the Prins Reaction.These addition compounds weve at first hydrolysed to sec- or test-keto-alcohols respectively and then dehydrated to methyl heptenone under appropriate conditions in good yield. The dehydration of 6-methyl-5-hydroxy-2-heptanone was best carried out at 280-370°c by passing through a pyrex glass tube, packed with pumice catalyst containing phosphoric acid. 6-Methyl-6-hydroxy-2-hepta-none was dehydrated to 6-methyl-5-hepten-2-one with a trace of iodine. On the other hand, 6-methyl-6-hydroxy-2-heptanone acetate was subjected to pyrolysis at 450°c through a pyrex glass tube, filled with crushed glass in almost quantitative yield, giving 6-methyl-6-hepten-2-one. 6-Methyl-6-hydroxy-2-heptanone, reported by Verley in 1897, which was obtained by the hydration of methyl heptenone with 40-50% H2SO4, differed apparently from the hydrolygate of 6-methyl-6-hydroxy-2-heptanone acetate. The substance which was obtained by Verley's method, was supposed to be 2, 2-dimethyl-6-methyl-6-hydroxy-tetrahydro pyran. When 6-methyl-5-hydroxy-2-heptanone acetate was hydrolyged with alcoholic sodium hydroxide solution, 2-isopropyl-5-methyl-5-ethoxy-tetrahydrof uran and 6-methyl-5-hydroxy-2-heptanone were obtained. The f uran ring of the former could be opened easily to the latter keto-alcohol when it was boiled with dil. HCl.
  • 過安息香酸を重合開始剤としたメタクリル酸メチルの重合について
    寺田 宏
    1962 年 20 巻 2 号 p. 158-164
    発行日: 1962/02/01
    公開日: 2011/07/05
    ジャーナル フリー
    Polymerization of methyl methacrylate was carried out by using peroxybenzoic acid as a polymerization initiator. The velocity of polymerization was proportional to the square root of the concentration of peroxybenzoic acid. From the velocity constant of formation of free radical from peroxybenzoic acid, the activation energy was 15.4 kcal and it was far smaller than the activation energy of benzoyl peroxide. The concentration of methyl methacrylate and the velocity of polymerization were approximately proportinal. The av. degree of polymerization was also proportional to the concentration. The reaction of decomposition of peroxybenzoic acid in methyl methacrylate for formation of free radical and initiating the polymerization was only a part of the whole decomposition reaction of peroxybenzoic acid but larger part of methyl meth-acrylate was decreased by the polymerization. Estimation of av, degree of polymerization of the polymer indicated that the reaction of polymer radical and peroxybenzoic acid caused much of chain transference and this caused the lowering of av. degree of polymerization. The activation energy of this transfer reaction was about 6.6 kcal.
  • Eulan U 33の有効成分について
    松井 弘次, 太田 悦郎
    1962 年 20 巻 2 号 p. 165-169
    発行日: 1962/02/01
    公開日: 2011/07/05
    ジャーナル フリー
    From a new Bayer's moth-proof agent, Eulan U 33, two effective substancesFrom a new Bayer's moth-proof agent Eulan U 33, two effective substances(1) (the main ingredient, C13H8O3NSCl5, mp. 137°c) and (2) (a by-product, C13HG O3NSCl7, mp. 196°c) were isolated. (1) and (2) showed behaviors very close to each other and both were decomposed with caustic alkali to give an amine (3) (C12H7ONCl4, mp. 98°c) and an amine (4) (C12H5ONCl6, mp. 123°c), respectively. (3) and (1) were found to be 4, 5, 2', 4'-tetrachloro-2-aminodiphenyl ether and its condensation product with chloromethanesvlfonyl chloride, chloromethan-esulfo-2-(2', 4'-dichchlorophenoxy)-4, 5-dichloroanilide, respectively. (4) and (2) were found to be a hexachloroaminodiphenyl ether and its amide of chloro-methanesulf onic acid, respectively.
  • ビストリアジルアミノスチルベン系ケイ光染料水溶液の日光に対する安定性
    野口 為彦, 前川 清二
    1962 年 20 巻 2 号 p. 170-173
    発行日: 1962/02/01
    公開日: 2011/03/01
    ジャーナル フリー
    It is already known that the aqueous solution of stilbene-type fluorescent dye is unstable against the sunlight and there is a report on a few stilbene derivatives that this was due to cis-traps geometrical isomerization by the ultraviolet light. In this experiment, one of the representative product from bistriazinyl-aminostilbene-type fluorescent dyes having value for practical use has been investigated in order to prevent the phenomenon of deterioration by light. The result indicated that some knowledge was obtained for the relation between the effect of time of exposure to sunlight and the photochemical change of aqueous solution of fluorescent dye as well as the effect of concentration of aqueous solution of fluorescent dye.
  • ω-クロルカルボン酸のアンモノリシス
    高木 行雄
    1962 年 20 巻 2 号 p. 174-176
    発行日: 1962/02/01
    公開日: 2010/06/28
    ジャーナル フリー
    Ammonolysis of ω-chloroenanthic acid and ω-chloropelargonic acid was carried out in the presence of 25% aqueous ammonia + ammonium salt. When ammonium carbonate was comployed, the yield of ω-aminocarboxylic acid was good with the lower mole ratio of ammonia/ω-chlorocarboxylic acid and by-product (mainly ω, ω'-iminodicarboxylic acid) was small amount. For increasing the mole concentration of ammonia in liquid phase, using of as much as possible of larger volume ratio (vol. of total raw materials in the autoclave/capacity of autoclave) and adjusting of suitable reaction velocity gave better result when the reaction was carried out at lower temperature.
  • 熊田 誠
    1962 年 20 巻 2 号 p. 177-189
    発行日: 1962/02/01
    公開日: 2010/06/28
    ジャーナル フリー
  • 吉田 従教
    1962 年 20 巻 2 号 p. 190-195
    発行日: 1962/02/01
    公開日: 2010/06/28
    ジャーナル フリー
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