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    • 4. 发明授权
    • Method for producing optically active 1-phenylethylamines
    • 光学活性1-苯基乙胺的制备方法
    • US6034278A
    • 2000-03-07
    • US194719
    • 1998-12-17
    • Walter MerzMartin LittmannUdo KraatzChristoph Mannheims
    • Walter MerzMartin LittmannUdo KraatzChristoph Mannheims
    • C07B53/00C07C209/88C07C211/27C07C211/29C07C209/00
    • C07C209/88
    • The invention concerns a new method for producing optically active 1-phenylethylamines, wherein (a) racemic 1-phenylethylamines are reacted with (S)-(-)-N-phenylcarbamate lactic acid in the presence of an aliphatic or aromatic hydrocarbon and in the presence of a lower aliphatic alcohol, wherein the reaction components are measured so that for every mole of racemic amine, between 0.25 and 0.5 mole of (S)-(-)-N-phenylcarbamate lactic acid are present, the reaction mixture is then concentrated at a liquid-phase temperature of up to 40.degree. C., the resulting solid product is separated, treated with diluted, aqueous alkaline lye in the presence of a hydrocarbon, and the respective (R)-amine is isolated by distillation from the organic phase, and if necessary, (b) the mother liquor remaining after the separation of the solid product is reacted in the presence of a lower aliphatic alcohol with (S)-(-)-N-phenylcarbamate lactic acid, wherein the reaction components are measured so that the molar quantity of (S)-(-)-N-phenylcarbamate lactic acid is twice as great as the quantity of (R)-amine still remaining in the mother liquor, the reaction mixture is then concentrated at a liquid-phase temperature of up to 40.degree. C., the resulting solid product is separated and the (S)-amine is isolated by distillation from the mother liquor.
    • PCT No.PCT / EP97 / 02988第 371日期1998年12月17日第 102(e)日期1998年12月17日PCT提交1997年6月9日PCT公布。 公开号WO97 / 49665 PCT 日期1997年12月31日本发明涉及一种用于制备光学活性1-苯基乙胺的新方法,其中(a)外消旋1-苯乙基胺与(S) - ( - ) - N-苯基氨基甲酸酯乳酸在脂肪族或 芳族烃和低级脂族醇的存在下,其中测量反应组分,使得对于每摩尔外消旋胺,存在0.25至0.5摩尔(S) - ( - ) - N-苯基氨基甲酸酯乳酸, 然后将反应混合物在高达40℃的液相温度下浓缩,分离得到的固体产物,在烃存在下用稀释的碱性碱水溶液处理,分离出(R) - 胺 (b)将固体产物分离后剩余的母液在低级脂族醇与(S) - ( - ) - N-苯基氨基甲酸酯乳酸的存在下反应, 其中测量反应组分 d,使得(S) - ( - ) - N-苯基氨基甲酸酯乳酸的摩尔量是母液中残留的(R) - 胺的量的两倍,然后将反应混合物以液 - 相温度高达40℃,分离得到的固体产物,并通过蒸馏从母液中分离出(S) - 胺。
    • 8. 发明授权
    • Process for the preparation of
2-(4-chlorophenylethyl)-2-tert.-butyl-oxirane
    • 2-(4-氯苯乙基)-2-叔丁基 - 环氧乙烷的制备方法
    • US4988829A
    • 1991-01-29
    • US373770
    • 1989-06-30
    • Paul FiedlerMartin LittmannManfred LentheAchim NoakGerd Siekmann
    • Paul FiedlerMartin LittmannManfred LentheAchim NoakGerd Siekmann
    • C07D303/08
    • C07D303/08
    • A process for making the known fungicide intermediate 2-(4-chlorophenyl ethyl)-2-tert.-butyloxirane of the formula ##STR1## comprising (a) mixing a solution of trimethylsulphonium bromide of the formula(CH.sub.3).sub.3 S.sup..sym. Br.sup..crclbar. (II) in a methanol/toluene mixture with preheated toluene and simultaneously distilling off a methanol/toluene mixture at a temperature between 65.degree. and 110.degree. C. until a suspension having a solids content between 10 and 70% by weight is formed, and(b) reacting the suspension of trimethylsulphonium bromide in toluene thus obtained with 1-(4-chlorophenyl)-4,4-dimethylpentan-3-one of the formula ##STR2## in the presence of solid potassium hydroxide, diethylene glycol and water at a temperature between 20.degree. and 120.degree. C., the amounts of the reaction components being such that per mole of 1-(4-chlorophenyl)-4,4-dimethylpentan-3-one of the formula (III) there are presentbetween 1 and 2 moles of trimethylsulphonium bromide of the formula (II),between 2 and 3 moles of solid potassium hydroxide and alsobetween 0.1 and 10% by weight of diethylene glycol and between 0.5 and 12% by weight of water, relative to 1-(4-chlorophenyl)-4,4-dimethylpentan-3-one of the formula (III).
    • 制备已知的杀真菌剂中间体式(I)的2-(4-氯苯基乙基)-2-叔丁基环氧乙烷的方法包括(a)将式(CH3)3S的三甲基锍溴化物 +)Br( - )(II)的甲醇/甲苯混合物中,同时在65-110℃的温度下蒸馏除去甲醇/甲苯混合物,直到固体含量为10至70% ,并且(b)使由此获得的甲苯中的三甲基锍溴化物的悬浮液与式(III)的1-(4-氯苯基)-4,4-二甲基戊-3-酮在存在 固体氢氧化钾,二甘醇和水,温度在20℃至120℃之间,反应组分的量使得每摩尔1-(4-氯苯基)-4,4-二甲基戊-3-酮为 式(III)中存在1至2摩尔式(II)的三甲基锍溴化物,2至3小时 固体氢氧化钾和0.1至10重量%的二甘醇和0.5至12重量%的水相对于式(I)的1-(4-氯苯基)-4,4-二甲基戊-3-酮, (三)。