首页> 外国专利> Gastrodin pharmaceutical intermediate 4-formylphenyl-2,3,4,6- O- acetyl -ß -D- glucopyranose glucoside synthesis method

Gastrodin pharmaceutical intermediate 4-formylphenyl-2,3,4,6- O- acetyl -ß -D- glucopyranose glucoside synthesis method

机译:天麻素医药中间体4-甲酰基苯基-2,3,4,6-O-乙酰基-ß-D-吡喃葡萄糖葡萄糖苷合成方法

摘要

#$%^&*AU2016102278A420170223.pdf#####ABSTRACT Gastrodin pharmaceutical intermediate 4-formylphenyl-2,3,4,60- acetyl -P -D- glucopyranose glucoside , comprising the following steps: the reaction vessel was added 0.062mola - substituting acetyl glucopyranosyl amine (2), 210ml toluene solution, 0.071-0.073mol hydroxybenzaldehyde (3) was dissolved 0.16mol sodium bisulfite solution, the two solutions were mixed, the solution temperature is raised to 40-45 C, allowed to stand for 30-36 h, toluene was distilled off under reduced pressure, the temperature of the solution is reduced to 10 15 C, the oil layer was separated, washed with potassium chloride solution for 9-11 times, added 300ml p-xylene solution, the solution temperature is raised to 60-65 C, maintain 60-90min, after decolorization with zeolite, the temperature of the solution is reduced to 3 - 5 C , to maintain 30-35h, white needle crystals was precipitated, filtered, washed with salt solution, washed with cyclohexane solution, dehydrated with dehydrating agent, recrystallized in nitroethane solution, got crystals 4-formylphenyl-2,3,4,6- 0- acetyl -P -D- glucopyranose glucoside .
机译:#$%^&* AU2016102278A420170223.pdf #####抽象天麻素医药中间体4-甲酰基苯基-2,3,4,60-乙酰基-P-D-吡喃葡萄糖葡萄糖苷,包括以下步骤:向反应容器中加入0.062mola-取代乙酰基吡喃葡糖胺(2),210ml甲苯溶液,0.071-0.073mol溶解羟基苯甲醛(3)0.16 mol亚硫酸氢钠溶液,将两种溶液混合,溶液温度升高到40-45℃,静置30-36小时,蒸出甲苯在减压下,溶液温度降至1015℃下,分离出油层,用氯化钾洗涤溶液9-11次,加入300ml对二甲苯溶液,溶液温度升至60-65 C,保持60-90min,之后用沸石脱色,溶液温度降至3-5 C维持30-35h,沉淀出白色针状晶体,过滤,用盐溶液洗涤,用环己烷溶液洗涤,用脱水剂脱水,在硝基乙烷溶液中重结晶,得到晶体4-甲酰基苯基-2,3,4,6- 0-乙酰-P -D-吡喃葡萄糖葡萄糖苷。

著录项

  • 公开/公告号AU2016102278A4

    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AU20160102278

  • 发明设计人 PENG FEI;

    申请日2016-12-24

  • 分类号C07H15/203;C07H1/00;

  • 国家 AU

  • 入库时间 2022-08-21 13:32:35

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