首页> 外国专利> Hydroxylamine azole cephalosporin propylene glycol drug intermediates D-a-tert-butoxycarbonylamino-a-(4-hydroxyphenyl)- acetic acid synthesis method

Hydroxylamine azole cephalosporin propylene glycol drug intermediates D-a-tert-butoxycarbonylamino-a-(4-hydroxyphenyl)- acetic acid synthesis method

机译:羟胺唑头孢菌素丙二醇药物中间体D-α-叔丁氧基羰基氨基-α-(4-羟苯基)-乙酸的合成方法

摘要

#$%^&*AU2016102153A420170216.pdf#####ABSTRACT Hydroxylamine azole cephalosporin propylene glycol drug intermediates D-a- tert-butoxycarbonylamino-ai-(4-hydroxyphenyl)acetic acid synthesis method, comprising the following steps: equipped with a stirrer, a reflux condenser, a thermometer, a reaction vessel was added 200ml with propionitrile solution, 0.06mol D-( I )-p-Hydroxyphenylglycine, 0.08mol sodium bromide solution, controlling the stirring speed at 160-190rpm, stirring time within 90-120min, 0.081-0.085mol tert-butoxycarbonyl bromide was slowly added in batches, controlling the solution temperature at 60--65 C, the reaction time is about 19-20h, diluted with 500ml potassium bromide solution, extracted with ethylenediamine 6-8 times, the aqueous layer was washed with oxalic acid solution, controlling pH of the solution to 5-6, potassium bromide solution was added to saturated, extracted with ethylenediamine for 4-5 times, the extract dehydrated with calcium chloride, vacuum distillation, the solvent was distilled off, the residue was added butanol solution, the solid was pulverized, filtered, got D-a-tert-butoxycarbonylamino-a-(4-hydroxyphenyl)-acetic acid.
机译:#$%^&* AU2016102153A420170216.pdf #####抽象羟胺唑头孢菌素丙二醇类药物中间体D-叔丁氧羰基氨基-ai-(4-羟苯基)乙酸的合成方法,包括以下步骤:用搅拌器,回流冷凝器,温度计,反应容器加200ml丙腈溶液,0.06molD-(I)-对羟基苯甘氨酸,0.08mol溴化钠溶液,控制搅拌速度在160-190rpm,搅拌时间在90-120min缓慢加入0.081-0.085mol叔丁氧羰基溴化物分批加入,将溶液温度控制在60--65 C,反应时间约19-20h,用500ml溴化钾稀释溶液,用乙二胺萃取6-8次,水层用草酸溶液洗涤,将溶液的pH值控制在5-6,加入溴化钾溶液至饱和,用硫酸镁萃取。乙二胺4-5次,提取液用钙脱水氯化物,真空蒸馏,蒸除溶剂,残留物加入丁醇溶液,将固体粉碎,过滤,得到D-α-叔丁氧基羰基氨基-α-(4-羟基苯基)-乙酸。

著录项

  • 公开/公告号AU2016102153A4

    专利类型

  • 公开/公告日2017-02-16

    原文格式PDF

  • 申请/专利号AU20160102153

  • 发明设计人 CHU DONGHONG;

    申请日2016-12-22

  • 分类号C07C269/04;C07C271/22;

  • 国家 AU

  • 入库时间 2022-08-21 13:32:33

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