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1. 发明授权

US3882177A Process for the preparation of DL-threo-1-(p-nitro-phenyl)-2-acetamino-1,3-propanediol 失效
标题翻译：制备DL-苏 - （对硝基 - 苯基）-2-乙酰氨基-1,3-丙二醇的方法
公开(公告)号：US3882177A
公开(公告)日：1975-05-06
申请号：US35771873
申请日：1973-05-07
申请人： EGYT GYOGYSZERVEGYESZETI GYAR
发明人： UJHIDY AUREL , SZOTYORI LASZLO , SZEPVOLGYI JANOS , HORVATH KAROLY , NAGY FERENC , ORBAN ISTVAN , SIMONYI ISTVAN
IPC分类号： C07C215/00 , C07C97/16
CPC分类号： C07C233/18
摘要： In a process for the preparation of DL-threo-1-(p-nitrophenyl)2-acetamino-1,3-propanediol from the isopropanol solution of DLthreo-1-(p-nitrophenyl)-2-acetamino-1,3-propanediol aluminiumalcoholate compounds formed in the Meerwein-PonndorfVerley reduction of p-nitro- Alpha -acetamino- Beta -hydroxypropiophenon via aqueous or aqueous-mineral acidic hydrolysis, evaporation and removal of the aluminium salt, the improvement that prior to or simultaneously with the separation of isopropanol the aluminium alcoholates formed in the reduction are hydrolyzed in the presence of the calculated amount or less, but not lower than 50 % of water, water vapour or of an equivalent amount of aqueous mineral acid solution, isopropanol is distilled out continuously, the powdery mixture of DL-threo-1-(pnitrophenyl)-2-acetamino-1,3-propanediol and aluminium oxide is treated to remove aluminium in the form of its double salt and optionally the hydrolysis is completed in this leaching step, and DL-threo-1-(p-nitrophenyl)-2-acetamino-1,3-propanediol is separated. This improved process can be carried out continuously with high yields and under optimum conditions, also making possible an almost complete recovery of isopropanol.
摘要翻译：在DL-苏 - （对 - 硝基苯基）-2-乙酰氨基-1（对 - 硝基苯基）-2-异丙基苯胺的异丙醇溶液中制备DL-苏 - （对硝基苯基）-2-乙酰氨基-1,3-丙二醇的方法中在Meerwein-Ponndorf-Verley中形成的3-丙二醇 - 醇铝化合物通过水或含水 - 无机酸性水解，蒸发和除去铝盐，还原对硝基-α-乙酰氨基-β-羟基 - 苯丙酮，改善了在分离异丙醇之前或同时，还原中形成的醇铝化物在计算量或更少但不低于50％的水，水蒸气或等量的无机酸水溶液的存在下水解，异丙醇被连续蒸馏出来，处理DL-苏 - （对 - 硝基苯基）-2-乙酰氨基-1,3-丙二醇和氧化铝的粉末混合物，以其双盐形式除去铝，任选的水解在这个浸出步骤中完成，而DL-thre 分离出邻-1-（对硝基苯基）-2-乙酰氨基-1,3-丙二醇。

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