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研究了将聚乙二醇用作相转移催化剂及其对亲核取代反应的改善.先将雌二醇经溴化制得2或4溴雌二醇,再分别在氯仿中以聚乙二醇(PEG400)作相转移催化剂(PTC)进行亲核取代反应制备2或4甲氧基雌二醇.发现其适宜条件为:反应温度60~65℃,搅拌反应时间1.5h,试剂比例底物为甲醇KOHPEG=120800.8,获得较高亲核取代产率:2甲氧基雌二醇66.7%及4甲氧基雌二醇70.3%,结果良好,操作简便.
The use of polyethylene glycol as a phase transfer catalyst and its improvement of the nucleophilic substitution reaction were studied. First estradiol obtained by bromination 2 or 4 bromo-estradiol, and then in chloroform to polyethylene glycol (PEG 400) for phase transfer catalyst (PTC) nucleophilic substitution reaction preparation 2 Or 4 methoxy oestradiol. The optimum conditions were as follows: the reaction temperature was 60-65 ℃, the reaction time was 1.5h, and the ratio of reagents was methanol KOHPEG = 120800.8, yielding higher nucleophilic substitution yield: 2-methoxyestradiol 66 .7% and 4-methoxyestradiol 70.3%, the results are good, easy to operate.