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Mercapto-acetaldehyde acetal(s) prepn. - by using chloro-acetaldehyde acetal(s) and synthetic intermediates from opt. continuous process

机译:巯基乙醛缩醛的制备-通过使用氯乙醛缩醛和opt的合成中间体。连续过程

摘要

Prepn. of mercaptoacetaldehyde acetals of formula (I) from haloacetals and mercapto cpds. comprises, a) mixing the chloroacetalaldehyde acetals (II) with aq. MSH soln. (m = alkali metal) in a reactor and heating to 80-100 deg.C b) removing the mixt. from the reactor as an organic phase and extracting (I) with aq. alkali, hydroxide soln, c) form the alkali metal salts of (I) solution, d) retwining the organic phase with unreacted (II) to the reactors, d) neutralising the aq. soln. of alkali salts of (II) and e) purifying (I) by distillation. R1, R2 = 1-2C alkyl, or R1+R2 = CH2CH2 or CH2CH(CH3). Cpds. (I) where R1 and R2 are present as R1+R2 are new. Pref. the MSH soln. is at pH 8-95. The process is carried out under a pressure of 0.1-0.2 mPa, in a water immiscible organic solvent which does not react with starting materials or prods. USE/ADVANTAGE - (I) are intermediates in the prepn. of pharmaceuticals, medicines and aromatic substances. The process may be continuous and gives good yields.
机译:准备式(I)的巯基乙醛缩醛由卤代缩醛和巯基cpds得到。包括:a)将氯乙醛缩醛(II)与水溶液混合。 MSH溶液。 (m =碱金属)在反应器中并加热至80-100℃b)除去混合物。从反应器中将其作为有机相并用饱和碳酸氢钠水溶液萃取(I)。碱,氢氧化物溶液,c)形成(I)溶液的碱金属盐,d)将未反应的(II)有机相再沉淀到反应器中,d)中和水溶液。 soln。 (II)的碱金属盐和e)通过蒸馏纯化(I)。 R1,R2 = 1-2C烷基,或R1 + R2 = CH2CH2或CH2CH(CH3)。 Cpds。 (I)R1和R2作为R1 + R2存在的地方是新的。首选MSH溶液。 pH值为8-95。该方法在不与原料或产物反应的与水不混溶的有机溶剂中,在0.1-0.2mPa的压力下进行。使用/优势-(I)是制备中的中间体。药品,药品和芳香物质。该过程可以是连续的并且提供良好的产率。

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