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Fluorouracil drug intermediates 1-benzyl-5-amino uracil phthalocyanine synthesis method

机译:氟尿嘧啶药物中间体1-苄基-5-氨基尿嘧啶酞菁的合成方法

摘要

#$%^&*AU2016102282A420170223.pdf#####ABSTRACT Fluorouracil drug intermediates 1 -benzyl-5 -amino uracil phthalocyanine synthesis method, comprising the following steps: equipped with a stirrer, thermometer and reflux condenser, the reaction vessel was added 0.23mol 1-amino-phthalide (2), 0.26-0.28mol 5-aminouracil, 0.31mol stannous chloride, 230ml cyclohexane solution, controlled stirring speed at 130-170 rpm, 0.13 mol sodium sulfite solution was added in batches, stirred for 5-7 h, filtered, and the filtrate was concentrated under reduced pressure , distilled off the cyclohexane, 630ml potassium chloride solution was added, the precipitated solid was filtered, washed with saline solution, dehydrated with dehydrating agent, added into acetonitrile solution, the solution temperature is raised to 60-65 C, after 60-80min, filtration, recrystallized from nitromethane solution, got crystals of 1 -benzyl-5-amino uracil phthalocyanine .
机译:#$%^&* AU2016102282A420170223.pdf #####抽象氟尿嘧啶药物中间体1-苄基5-氨基尿嘧啶酞菁的合成方法,包括以下步骤:装有搅拌器,温度计和回流冷凝器,反应向容器中加入0.23mol 1-氨基邻苯二甲酸酯(2),0.26-0.28mol5-氨基尿嘧啶,0.31摩尔氯化亚锡,230毫升环己烷溶液,在130-170 rpm下控制搅拌速度,0.13 mol亚硫酸钠溶液分批加入,搅拌5-7小时,过滤,并过滤滤液。减压浓缩,蒸除环己烷,加入630ml氯化钾溶液,沉淀出的固体为过滤,用盐水溶液洗涤,用脱水剂脱水,加入乙腈溶液中,溶液温度升至60-65°C,60-80min后,过滤,从硝基甲烷中重结晶溶液,得到1-苄基-5-氨基尿嘧啶酞菁晶体。

著录项

  • 公开/公告号AU2016102282A4

    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AU20160102282

  • 发明设计人 PENG FEI;

    申请日2016-12-24

  • 分类号C07D405/04;

  • 国家 AU

  • 入库时间 2022-08-21 13:32:35

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