YAKUGAKU ZASSHI
Online ISSN : 1347-5231
Print ISSN : 0031-6903
ISSN-L : 0031-6903
75 巻 , 4 号
選択された号の論文の35件中1~35を表示しています
  • 錠剤の崩壞時間について
    長谷川 淳, 池田 憲
    1955 年 75 巻 4 号 p. 359-363
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    Tablets were manufactured with the same base but varying the kind, concentration, and amount of the binding agent, and pressure added, and their influence on the crumbling time was examined. In this case, use of sodium arginate as the binding agent resulted in the tablets not crumbling in synthetic gastric juice but rapidly crumbling in synthetic enteric juice and effected enteric coating. Sulfathiazole and Benadryl tablets were prepared with sodium arginate as the binding agent and their blood level was examined after administration of such tablets. The rate of excretion of sulfathiazole was so small that the effect could not be observed but the effect was clearly observed with Benadryl, the maximum blood level being maintained for 5-6 hours.
  • ビニルピロリドンの過酸化水素及びアンモニアによる水溶液重合について
    大津 隆行, 的場 啓子, 菊地 茂行, 平尾 一郎
    1955 年 75 巻 4 号 p. 364-367
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    When polyvinylpyrrolidone is used as the substitute plasma, it should possess a molecular weight of 30, 000 to 50, 000. Therefore, polymerization of vinylpyrrolidone in aqueous solution with hydrogen peroxide and ammonia as catalysts was examined to find the influence of various factors. It was thereby found that the molecular weight of polyvinylpyrrolidone decreased with the increase in the concentration of hydrogen peroxide, and increased with the increase in the concentration of ammonia. The presence of oxygen was found to inhibit the polymerization and the molecular weight of the polymer formed was found to be markedly low. Kinetic study of the polymerization of vinylpyrrolidone with hydrogen peroxide and ammonia as catalysts gave the value of 10.7±1.7kcal./mole as the activation energy. This value agrees well with the existing value for the polymerization of vinyl monomer in aqueous solution with hydrogen peroxide and a ferrous salt and the polymerization with hydrogen peroxide and ammonia was considered to proceed under the same redox mechanism.
  • ポリビニルピロリドンの分別と粘度測定結果について
    大津 隆行, 的場 啓子, 菊地 茂行, 平尾 一郎
    1955 年 75 巻 4 号 p. 368-371
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    Polyvinylpyrrolidone, used as the substitute plasma, is said to be effective when the molecular weight is around 30, 000 to 50, 000, and the inclusion of lower or higher molecules is thought to give adverse effect as a substitute plasma. The polymer obtained by the polymerization of vinylpyrrolidone with hydrogen peroxide and ammonia catalyst was extracted with acetone at a room temperature and fractionated by reprecipitaton from aqueous solution with acetone, obtaining a distribution curve for molecular weights.
    On the other hand, distribution curve of molecular weights was also obtained by the same method from the polyvinylpyrrolidone marketed by the German Bayer and the two curves were found to be very similar. These results show that the extraction of low molecular polymers with a solvent like acetone is effective in obtaining polyvinylpyrrolidone of high homogeneity. Polyvinylpyrrolidone is known to take a coiled form in a solution that its viscositic characteristics in dilute aqueous solution were also examined and it was observed that the Huggins' viscosity constant, k', markedly changes with the degree of polymerization.
  • 藤田 穆, 廣瀬 良男, 古川 佳也, 窪 茂, 佐々木 義郎, 大森 重徳, 中島 哲郎, 淵上 財棋, 黒木 和子
    1955 年 75 巻 4 号 p. 371-374
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    Some derivatives of undecanoic acid with substituted phenyl group in the ω-position and brassylic acid with the acid amide combination in one of the two carboxyl groups were prepared. Antibacterial tests of these compounds showed that some of them possessed interesting behavior against virus infections while their action against bacteria was not significant.
  • シオール型Vitamin B1誘導体について その5 O, S-DiacylthiamineとThiolまたはAmineとの反応
    川崎 弌
    1955 年 75 巻 4 号 p. 374-378
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    O, S-Diacylthiamines, such as O, S-diacetylthiamine (DAT), O, S-dibenzoylthiamine (DBT), and O-benzoyl-S-acetylthiamine, react with compounds possessing an active thiol group, such as glutathione, cysteine, and β-aminoethanethiol, and the S-acyl group easily undergoes transacylation. The S-acetyl group in DAT also undergoes transacetylation with amines, such as aniline. These facts seem to offer some suggestions as to the action mechanism of thiamine.
  • 置換安息香酸による石炭酸のアシル化
    中沢 浩一, 馬場 茂雄
    1955 年 75 巻 4 号 p. 378-381
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    Fifteen kinds of mono-substituted benzoic acid possessing OCH3, OH, CH3, Cl, or NO2 in the ortho-, meta-, or para-position of the carboxyl were reacted respectively with phenol, in the presence of polyphosphoric acid. It was thereby found that the nuclear substitution became difficult in the order of OCH3, OH, CH3, H, Cl, and NO2, and the influence of substituents on the nuclear substitution appeared more clearly in the ortho- and para-substituted acids. Nitrobenzoic acids were most resistant to substitution.
  • 2-Salicylidenehydrazono-4-thiazolidone関連化合物の合成及び抗菌作用その1
    谷山 兵三, 田中 幸夫, 内田 譽
    1955 年 75 巻 4 号 p. 382-387
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    In order to prepare chemotherapeutics for tubercle bacilli, relationship between chemical structure and antibacterial action was examined. It was revealed by in vitro tests that 2-salicylidenehydrazono-4-thiazolidone and its 5-methyl derivative possessed powerful antituberculous action. As compounds related to the above, various arylidenehydrazono-4-thiazolidones and their 5-methyl derivatives were prepared and their antibacterial action was tested but all showed only a weak activity. These compounds all possess the action group=N-N=CH-R (R=aryl) but lack the hydroxyl in the benzene ring of the aryl group that the antibacterial activity has been weakened. It was confirmed that the presence of thiazolidone or thiazole ring in the group bonded to the terminal nitrogen was necessary in increasing the antibacterial activity. A few new observations were obtained in the synthetic method for these compounds.
    In the condensation of aldehyde thiosemicarbazones and the esters of α-hologenated-fatty acids by the usual method, the presence of a neutralization agent, such as sodium acetate or N-ethylpiperidine, was found to give a good yield. There is another method of reacting α, β-dichlorovinyl ethyl ether to the thiosemicarbazone and the newly discovered present method of reacting aldehydes with 2-hydrazono-4-thiazolidone hydrochloride or the hydrochloride of its 5-methyl derivative.
  • 2-Salicylidenehydrazono-4-thiazolidone関連化合物の合成及び抗菌作用 その2
    谷山 兵三, 田中 幸夫, 内田 譽
    1955 年 75 巻 4 号 p. 387-391
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    The compounds possessing structures related to 2-salicylidenehydrazono-4-thiazolidone (I) and its 5-methyl derivative (II) were prepared and their antibacterial action in vitro was examined. 2-[(β-Hydroxy-α-naphtylmethylene) hydrazono]-4-thiazolidone, 2-o-acetoxybenzylidenehydrazono-4-thiazolidone, and their 5-methyl derivatives showed somewhat poorer action than (I) or (II) but still retained the antibacterial activity. However, the compounds with hydroxyl in the benzene ring situated in the meta- or para-position of the action group, =N-N=CH-, such as 2-m- or 2-p-hydroxybenzylidenehydrazono-4-thiazolidone and their 5-methyl derivatives, were entirely devoid of such action. Ten kinds of such compounds in which the hydroxyl in the ortho-position had been substituted with an alkoxyl (methoxy, ethoxy, propoxy, isopropoxy, and butoxy), and their respective 5-methyl derivatives also lacked such antibacterial activty. The foregoing results indicate that the following conditions must be fulfilled in order that the compounds show antibacterial activity.
    1) Hydroxyl in the benzene ring must be situated ortho to =N·N=CH.
    2) Hydroxyl must be in a free form or in a form that will easily change to the free hydroxyl.
    These compounds were obtained by the reaction of aldehyde thiosemicarbazones and ethyl chloroacetate or ethyl α-bromopropionate, the presence of a neutralization agent, such as sodium acetate or N-ethylpiperidine, giving a good yield of the product.
  • p-位置換benzal化合物
    卯尾田 秀隆, 谷崎 太吉
    1955 年 75 巻 4 号 p. 391-395
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    In order to improve solubility in water of tuberculosis drugs of thioacetazone series, the corresponding aldehydes and 1-amino-hydantoin or 1-amino-2-thiohydantoin were reacted (method A), or the corresponding aldehydes and ethyl N1-carbamoyl- or thiocarbamoyl-hydrazinoacetate were reacted and derived first to the chain-form azomethine compounds (cf. Table II), which were then heated with dilute mineral acids (method B). By the method A or B, N-benzal-1-aminohydantoin and -1-amino-2-thio-hydantoin, possessing CH3CONH-, CH3O-, C2H5SO2-, HOOC-, and NO2- in the para-position, which may be assumed as the cyclic semicarbazone or thiosemicarbazone, and the corresponding bis-form compounds of terephthalaldehyde, and p, p'-diformyldiphenyl sulfone, were prepared (cf. Table I).
  • サントニン合成におけるMichael縮合
    三木 卓一
    1955 年 75 巻 4 号 p. 395-399
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    The Michael-type condensation of diethyl malonate, methyl cyanoacetate, methyl cyanopropionate, or ethyl acetoacetate with 3-oxo-4, 9-dimethyl-1, 2, 3, 7, 8, 9-hexahydronaphthalene, possessing a linear extended dienone system, results in the specific formation of an equatorial side chain at C6-position. This configuration is the same as that at C7-position of natural santonin and a grave difficulty has been overcome for the synthesis of santonin by this discovery.
  • 11-Norsantoninの合成
    三木 卓一
    1955 年 75 巻 4 号 p. 399-402
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    Starting with 3-oxo-11-noreusanton-4-enic acid, 11-norsantonin was synthesized by the same method as in the preparation of the cis-lactone isomer of santonin and its resolution to optically active substances was carried out.
  • 二酸化セレンによるサントニン型Dienone環の新合成法
    三木 卓一
    1955 年 75 巻 4 号 p. 403-406
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    Application of selenium dioxide to monoënone ring compound in glacial acetic acid and pyrolysis of the selenium compound thereby obtained to obtain cross-conjugated dienone ring compound is introduced as a new synthetic reaction and compared with other methods.
  • 二酸化セレンによるサントニン型ラクトンの新合成法
    三木 卓一
    1955 年 75 巻 4 号 p. 407-409
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    Boiling a solution of 3-oxo-eusantona-1, 4-dienic acid homolog dissolved in glacial acetic acid with selenium dioxide for a few hours results in hydroxylation of the C6-position with concurrent lactonization to give a trans-lactone as in santonin. The applicability of this new reaction was examined. The use of mercuric acetate, in place of selenium dioxide, was found to yield cis-lactone compound.
  • 11-Norsantoninの合成別法と立体化学
    三木 卓一
    1955 年 75 巻 4 号 p. 410-411
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    Dehydrogenation of methyl 3-oxo-11-noreusanton-4-enate (II) with selenium dioxide to dienone compound (III) and its saponification followed by oxidation with selenium dioxide yields 11-norsantonin (V), which was found to be identical with the previously reported 11-norsantonin. Further stereochemical considerations led to the assumption that (V) is a cis-lactone compound.
  • サントニンのラクトン環に関する研究
    三木 卓一
    1955 年 75 巻 4 号 p. 412-415
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    l-α-Santonin was derived to pure l-α-santoninic acid, methyl l-α-santoninate, and l-α-santoninonitrile. Four isomers of rac-santoninic acid were also synthesized and rac-α-santoninic acid thereby obtained was resolved into optically active compounds by treatment with brucine. Treatment of santonin C and D, possessing cis-lactone, with zinc dust and acetic acid easily effects reductive cleavage of the lactone ring to form 3-oxo-eusantona-1, 4-dienic acid (XIIIa) and its C11-epimer (XIIIb). α- and β- Santonin possessing a trans-lactone do not undergo this change under the same conditions. This reaction mechanism was discussed.
  • サントニンのC11位の立体配置について
    三木 卓一
    1955 年 75 巻 4 号 p. 416-417
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    Based on the facts that the lactonization velocity of α-santoninic and β-santoninic acids differs, that decarboxylation of 11-carboxysantonin specifically yields α-santonin, and that the lactone ring in santonin was isosteric with the D ring in steroids, steric conformation of the C11-position was discussed, utilizing the conformational analysis initiated by Barton. This has finally resolved the one doubt remaining in the question of the relative conformation of santonin.
  • 愛甲 軍雄, 猿渡 健市
    1955 年 75 巻 4 号 p. 418-420
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    Bis (β-chloroethyl) amine reacts with acyl chlorides in benzene to form its acylamide compounds which, when left in the open, absorb one mole of water and convert to β-chloroethyl-β′-acyloxyethylamine hydrochlorides. Reaction of bis (β-chloroethyl) amine respectively with chloroacetyl, benzyl, and acetyl chloride yielded N-bis (β-chloroethyl)-chloracetamide, -benzamide, and acetamide which absorbed 1 mole each of water and changed respectively to β-chloroethyl-β′-chloroacetoxy-, -benzoxy-, and -acetoxy-ethylamine hydrochloride. Rearrangement velocity of N-bis (β-chloroethyl) acetamide in 80% acetone was measured.
  • 各種TBP反応陽性物質のキノン処理反応について
    鈴木 周一
    1955 年 75 巻 4 号 p. 420-423
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    In order to prove the reaction course of the quinone treatment against pyrogen, 32 kinds of substances giving positive TBP reaction were submitted to quinone treatment as described in the preceding paper. It was thereby clarified that substances containing pyrogen, as well as many of the structurally known pyrogenic substances and TBP-positive substances behaved in the same manner as pyrogen against the quinone treatment, as evidenced by the following results:
    1) Thirty-two kinds of TBP-reaction positive substances, such as the pyrogen culture filtrate, pyrogenic glucose parenteral solution, organic amines such as pyridine and guanidine, and biological constituents such as thymine and pantothenic acid, were removed by the quinone treatment, as in the case of pyrogen.
    2) Digestion of the activated carbon used for the quinone treatment with warm water showed that the TBP-positive substances were invariably transited to the aqueous phase and this has confirmed that there is no inconsistency in the writer's assumption regarding the liberation reaction of pyrogen×.
  • Furfural Diacetateの硝化に於ける中間附加化合物に関する研究 その1
    木村 隆一
    1955 年 75 巻 4 号 p. 424-426
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    1) The intermediate product obtained by the nitration of furfural diacetate with nitric acid and acetic anhydride yielded three kinds of crystals melting respectively at 114.5-115.5°, 106-107°, and 105-105.5°. Analytical and other examinations pointed out that they were all furfural diacetate with nitro and acetoxyl groups and they were designated respectively as α-, β-, and γ-nitro-acetin diacetate.
    2) Deacetoxylation of nitro-acetin diacetate was examined from various angles and it was found that it could be effected with weak inorganic alkalis, such as sodium acetate, not necessarily requiring pyridine or dimethylaniline, to form 5-nitrofurfural diacetate in a good yield.
  • Furfural Diacetateの硝化に於ける中間附加化合物に関する研究 その2
    木村 隆一
    1955 年 75 巻 4 号 p. 427-429
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    Examinations of the α-, β-, and γ-nitro-acetin diacetates, formed as the intermediate adducts during the nitration of furfural diacetate were made through X-ray powder photography, ultraviolet absorption spectra, and microscopic observations. It was thereby confirmed that α- and β-compounds are dimorphic and that the γ-compound possesses a structure somewhat different from those of α- and β-compounds. Further, transition phenomena between α- and β-compounds were clarified.
  • トリエチルアミン-水系の気液平衡
    石黒 武雄, 柳生 正見, 生島 正生, 中沢 太一
    1955 年 75 巻 4 号 p. 430-433
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    Fractional distillation of a mixture of triethylamine and water was carried out by the Podbielniak's apparatus and the presence of an azeotropic mixture was confirmed from its fractionation curve. The azeotropic mixture boils out at 75.3-75.6° and its composition was determined as 90.0% amine. Vapor-liquid equilibrium distillation on the same system was then carried out with the Othmer apparatus and the boiling point curve of the triethylamine-water system was drawn up. As a result, binary equilibrium diagram of the triethylamine-water system at temperatures between 0° and 100° was completed.
  • α-Picoline-H2O-NaOH系の相互溶解度
    石黒 武雄, 亀谷 富士夫, 古座谷 醇
    1955 年 75 巻 4 号 p. 434-438
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    In order to measure the mutual solubility of a ternary system of α-picoline, water, and sodium hydroxide system at 0, 30, 60, and 90°, the amount of the three components in the upper and lower layers in an equilibrium state at each temperature was quantitatively determined and the mutual solubility curve was drawn on a triangular graph. Dehydration of α-picoline by sodium hydroxide increases with the rise of temperature, i.e. the conentration of α-picoline present with a definte concentration of sodium hydroxide increases with the rise of temperature. When the temperature is definite, the concentration of α-picoline in the upper layer becomes greater as the concentration of sodium hydroxide in the lower layer becomes greater. In other words, the mutual solubility of the α-picoline-water-sodium hydroxide system decreases with the increase of the temperature.
  • 鍛冶 健司, 長島 弘, 二ノ井 襄, 花田 俊彦
    1955 年 75 巻 4 号 p. 438-441
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    By heating phenyl- and p-nitrophenyl-ω-diazoacetone in ethanol with thiourea, 4-benzyl- and 4-(p-nitrobenzyl)-2-aminothiazole were obtained in a comparatively good yield. In general, the reaction of aryl-ω-diazoacetone and thiourea may be termed a simplified method of the Hantsch's thiazole cyclization.
  • フェニルピラゾロンのスルフォンアミド誘導体に就いて
    板野 公平
    1955 年 75 巻 4 号 p. 441-444
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    Five kinds of 1-(p-sulfamylphenyl)-5-pyrazolone derivatives were synthesized from p-sulfamylphenylhydrazine. These derivatives were combined with p-diethylaminoaniline to obtain the corresponding pyrazolone-azomethine dyes whose spectrophotometric absorption was measured in methanol.
  • 9-OximinodehydroabietinsäuremethylesterのBeckmann転位 その2
    太田 道敏
    1955 年 75 巻 4 号 p. 445-449
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    The acid, b.p3 193-195°, formed by the decomposition of the lactam with conc. hydrochloric acid (cf. Fig 2), separates into two kinds of acids, one (VII) of m.p. 120-122°, [α]D29: +30.7°, and the other (VIII) of m.p. 111-113°, [α]D28: +16.7°, by purification of its anilide. (VII) transits to another (VI) of m.p. 189.5-191°, [α]D28: +71.3°, when treated with potassium hydroxide, and (VI) reverts back to (VII) when heated with dil. hydrochloric acid. The analytical values of (VI), (VII), and (VIII) all correspond to those of C11H16O4, a monobasic acid and a γ-lactone according to infrared spectral analyses. Reduction of the methyl esters of (VI) and (VII) with lithium aluminum hydride yields the identical triol, m.p. 157-159°, [α]D14: +45.5°. The same treatment of the methyl ester of (VIII) affords a triol of m.p. 102-103°, [α]D15: -0.6. Both these triols possess two hydroxyls which can be acetylated. Dehydrogenation of (VI) and (VIII) with selenium yields 1, 2, 3-trimethylbenzene. The foregoing experiments suggest that (VI) and (VII) would be represented by one of the A and B formulae shown in Fig. 2 and (VIII) is assumed to be a stereoisomer of (VI) or (VII).
  • Diphenyl誘導体のHydrazine Hydrateに依る開裂反応 その1
    富田 眞雄, 井川 健二
    1955 年 75 巻 4 号 p. 449-453
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    The diphenyl ether derivatives possessing a nitro group in the ortho-position undergo hydrazinolysis by the action of hydrazine hydrate at an ordinary pressure. The three kinds of methyl o-nitro-diphenyl ether-carboxylate (I) undergo cleavage of the ether-bond oxygen constituting the diphenyl ether and form o-nitrophenylhydrazine (II) and hydroxybenzoic acid hydrazide (III). (II) further undergoes dehydration and is isolated as 1-hydroxybenzotriazole (IIa) and only a minute amount of the objective o-nitrodiphenyl ether-carboxylic acid hydrazide (IV) is obtained. Similar cleavage occurs in 2-nitrodiphenyl ether-carboxylic acid (V) and 2-nitro-4′-chlorodiphenyl ether but 2-nitrodiphenyl ether and 2-nitromethyldiphenyl ether (VI) do not undergo this cleavage reaction by hydrazine hydrate.
  • Diphenyl Ether誘導体のHydrazide Hydrateに依る開裂反応 その2
    井川 健二
    1955 年 75 巻 4 号 p. 453-456
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    Occurrence of hydrazinolysis in 4-nitrodiphenyl ether derivatives was found to be in following cases. When the substituent present in the benzene ring not possessing the nitro group is an ester of a carboxylic acid, and is in the ortho-position to the oxygen bond constituting the diphenyl ether linkage, then the cleavage occurs at ordinary pressure, and when at meta- or para-position, the reaction occurs only when carried out under a high pressure. When the said substituent is a free carboxylic acid, the cleavage occurs only under a high pressure, whether the group is in ortho-, meta-, or para-position. When the substituent is a methyl, the cleavage does not occur, either under ordinary or high pressure. 4-Nitrodiphenyl ether itself yields the corresponding 4-aminodiphenyl ether by the high pressure reaction.
  • Diphenyl Ether誘導体のHydrazine Hydrateに依る開裂反応 その3
    井川 健二
    1955 年 75 巻 4 号 p. 457-460
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    3-Nitrodiphenyl ether derivatives do not undergo cleavage of the ether-bond oxygen by hydrazine hydrate, irrespective of the kinds of the substituent present in the benzene ring not possessing the nitro group or of the position of such a substituent, and only the reduction of the nitro group occurs, forming the corresponding 3-aminodiphenyl ether derivatives. 2, 4-Dinitrodiphenyl ether derivatives (VI) undergo cleavage' by hydrazine hydrate and afford 2, 4-dinitrophenylhydrazine (VII), and a small amount of 1-hydroxy-6-nitrobenzotriazole (VIIa) formed by the dehydration of (VII) and p-hydroxybenzene derivative (VIII).
  • 井川 健二
    1955 年 75 巻 4 号 p. 460-461
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    Three kinds of new diphenyl ether-carboxylic acid hydrazide derivatives possessing an amino group in the ortho-position, not described in any literature as yet, were prepared. They are 2-aminodiphenyl ether-2′-carboxylic acid hydrazide (III), -3′-carboxylic acid hydrazide (IV), and -4′-carboxylic acid hydrazide (V).
  • dl-ジセントリン合成に於けるPschorr反応の検討
    萩庭 丈壽, 村越 勇
    1955 年 75 巻 4 号 p. 462-464
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    In preparing dicentrine by the Pschorr reaction of 1-(3′, 4′-dimethoxy-6′-amino)-benzyl-2-methyl-6, 7-methylenedioxytetrahyroisoquinoline, the concurrent use of methanol or ethanol with copper dust as a reduction agent gives a better yield. The use of hypophosphoric acid as the reduction agent results in comparatively large formation of a deaminated compound and occurrence of an unwarranted side-reaction.
  • 加納 日出夫, 牧角 徳夫
    1955 年 75 巻 4 号 p. 465-466
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    In the reaction of methyl α-chloroethyl ketone (I) and an aqueous solution of sodium cyanide, reaction conditions (molar ratio of the starting materials and reaction temperature) and the formation ratio of the reaction products, acetopropionitrile (II) and α, β-dimethylglicidic nitrile (III), were examined (cf. Table I). (III) reacts with a carbonyl reagent to form a diacetyl derivative, and with ammonia to form 2, 5-dicyanotetramethylpiperazine (V). Pyrolysis or hydrolysis of (V) yields tetramethylpyrazine (VI) and treatment of (V) with nitrous acid yields a dinitroso compound (VII).
  • 8-メチルアカセチン-5,7-ジメチルエーテル及び8-(β-カルボキシエチル)-5,7,4´-トリメトキシフラボンの新合成法
    中沢 浩一, 松浦 信
    1955 年 75 巻 4 号 p. 467-469
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    8-Methylacacetin 5, 7-dimethyl ether (V) and 8-(β-carboxyethyl)-5, 7, 4′-trimethoxyflavone (XIII) were synthesized through flavone or chalcone. Condensation of C-methylphloroglucinol dimethyl ether (I) and p-methoxycinnamoyl chloride (II), in the presence of aluminum chloride afforded the flavanone (III), which was derived to (V) by treatment with N-bromosuccinimide and then with collidine, and the chalcone (IV), which was also derived to (V) by acetylation, bromination, and treatment with ethanolic potassium hydroxide. Condensation of the ester (IX) of 1-(β-carboxyethyl)-2-hydroxy-4, 6-dimethoxybenzene (VIII) with (II) gave the chalcone (X) which was derived to (XIII) by acetylation, bromination, and treatment with ethanolic potassium hydroxide.
  • 中沢 浩一, 松浦 信
    1955 年 75 巻 4 号 p. 469-470
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    The chalcones (I) and (II), derived from phloroglucinol, are almost quantitatively cyclized to the corresponding flavanones (III) and (IV) on being heated with 95-100% phosphoric acid for 5 minutes on a boiling water bath.
  • 野上 壽, 関口 慶二
    1955 年 75 巻 4 号 p. 471-473
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    A new method of making samples for thermal analysis of organic compounds was devised. The ratio of the components was changed by the volume of their solution in organic solvents and not by weighing. Its practical applications showed the method to be simple, rapid, and reliable.
  • 竹本 常松, 矢萩 和
    1955 年 75 巻 4 号 p. 473-474
    発行日: 1955/04/25
    公開日: 2010/02/19
    ジャーナル フリー
    Examination of the constituent of the leaves of Callistemon rigidus R. Br. (Myrtaceae) revealed the presence of cineol and a kind of triterpenoid, C30H48O3, m.p. 322°, [α]D14: +40°, which was found to be identical with melaleucin, the constituent of a bark of Melaleuca leucadendron L. (Myrtaceae), by mixed fusion and measurement of the infrared absorption spectrum. Its acetate, m.p. 298-299°, C32H50O4, methyl ester, m.p. 231-232°, C31H50O3, and acetate of methyl ester, m.p. 217-218°, C33H52O4, were also prepared.
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