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Perhexiline drug intermediates a-(2,2- diphenyl-vinyl) pyridine synthesis method

机译:哌克昔林药物中间体α-(2,2-二苯基-乙烯基)吡啶的合成方法

摘要

#$%^&*AU2016102318A420170223.pdf#####ABSTRACT Perhexiline drug intermediates a-(2,2-diphenyl-vinyl) pyridine synthesis method, comprising the following steps: equipped with a stirrer, a reflux condenser, a thermometer, a dropping funnel, a reaction vessel was added 1.56mol 1,1-diphenyl-2 (- pyridyl) ethylamine (2), 1.8-2.1mol hypochlorous acid phenyl ester solution (3), 300ml nitromethane solution, controlling the stirring speed at 150-190rpm, the solution temperature is raised to 80-85 C, reacted for 3-5h, the temperature of the solution is reduced to 45-50'C, potassium carbonate solution was added, the pH was adjusted to 9-10, the reaction continued stirring for 5-7h, the temperature of the solution is reduced to 10-15'C, the precipitated solid was suction filtered, washed with salt solution, washed with chlorobenzene solution, zeolite decolorization, stirred and reflux for 3-4h, dehydrated with dehydrating agent, recrystallized from p-xylene solution, got crystalsa -(2,2-diphenyl-vinyl) pyridine.
机译:#$%^&* AU2016102318A420170223.pdf #####抽象哌克昔林药物中间体α-(2,2-二苯基-乙烯基)吡啶合成方法,包括以下步骤:配备搅拌器,回流冷凝器,温度计,滴液漏斗,反应容器加入1.56摩尔1,1-二苯基-2(-吡啶基)乙胺(2),1.8-2.1摩尔次氯酸苯酯溶液(3),300ml硝基甲烷溶液,控制搅拌速度在150-190rpm,溶液温度为升至80-85 C,反应3-5h,溶液温度为还原至45-50'C,加入碳酸钾溶液,pH为调节至9-10,反应继续搅拌5-7h,温度将该溶液的温度降低至10-15'C,将沉淀的固体抽吸过滤,用盐溶液洗涤,用氯苯溶液洗涤,沸石脱色,搅拌并回流3-4h,用硫酸钠脱水脱水剂,在对二甲苯溶液中重结晶,得到结晶-(2,2-二苯基-乙烯基)吡啶。

著录项

  • 公开/公告号AU2016102318A4

    专利类型

  • 公开/公告日2017-02-23

    原文格式PDF

  • 申请/专利权人 XIAMEN KAI ER LI INFORMATION TECHNOLOGY CO. LTD;

    申请/专利号AU20160102318

  • 发明设计人 GUAN GENAN;

    申请日2016-12-25

  • 分类号C07D213/127;C07D213/16;

  • 国家 AU

  • 入库时间 2022-08-21 13:32:35

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