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3-(3-羟基-1-甲基丙氧基)-1-丁醇和3-(3-羟基丁氧基)-1-丁醇的合成及其工艺改进
引用本文:张青,张兴锴,田峰,孙铁民,季光辉.3-(3-羟基-1-甲基丙氧基)-1-丁醇和3-(3-羟基丁氧基)-1-丁醇的合成及其工艺改进[J].中国药物化学杂志,2008,18(1):38-39,43.
作者姓名:张青  张兴锴  田峰  孙铁民  季光辉
作者单位:1. 沈阳药科大学,制药工程学院,辽宁,沈阳,110016
2. 东北制药总厂,辽宁,沈阳,110026
摘    要:目的合成3-(3-羟基-1-甲基丙氧基)-1.丁醇(Ⅰ)和3-(3-羟基丁氧基)-1-丁醇(Ⅰ),并改进工艺提高产品纯度。方法以1,3-丁二醇为起始原料,通过硫酸催化双分子缩合、三苯甲基选择性保护、分离提纯、脱保护基4步反应得到目标化合物。结果与结论化合物Ⅰ的结构经。H.NMR13C-NMR谱确证,其含量经C-C测定,大于99.5%。化合物Ⅰ的纯度为90.0%,与文献相比纯度都有相应提高。

关 键 词:3-(3-羟基-1-甲基丙氧基)-1-丁醇  3-(3-羟基丁氧基)-1-丁醇  1  3-丁二醇  工艺改进
文章编号:1005-0108(2008)01-0038-02
收稿时间:2007-05-29
修稿时间:2007年5月29日

Synthesis and improvement of 3-(3-hydroxy-1-methylpropoxy)- 1-butanol and 3-(3-hydroxybutoxy)-1-butanol
ZHANG Qing,ZHANG Xing-kai,TIAN Feng,SUN Tie-min,JI Guang-hui.Synthesis and improvement of 3-(3-hydroxy-1-methylpropoxy)- 1-butanol and 3-(3-hydroxybutoxy)-1-butanol[J].Chinese Journal of Medicinal Chemistry,2008,18(1):38-39,43.
Authors:ZHANG Qing  ZHANG Xing-kai  TIAN Feng  SUN Tie-min  JI Guang-hui
Institution:School of Pharmaceutical Engineering, Shenyang Pharmaceutical University, Shenyang 110016, China
Abstract:To synthesis 3-(3-hydroxy-1-methylpropoxy)-1-butanol(Ⅰ) and 3-(3-hydroxybutoxy)-1-butanol(Ⅲ),and to improve its synthetic procedure.Methods The target compound were synthesized from 1,3-butandiol through 4-step reactions, including catalytic condensation by sulfuric acid, selective protection by triphenylchloromethane, separation and deprotection. Results and conclusion The structure of compoundⅠwas confirmed by 1H-NMR、13C-NMR, and its purity determined by GC was higher than 99.5%,purity of compound Ⅲ was 90.0%.
Keywords:3-(3-hydroxy-1-methylpropoxy)-1-butanol  3-(3-hydroxybutoxy)-1-butanol  1  3-butandiol  procedure improvement
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