目录
前言.................................................................3
1．1 医药中间体简介 ..................................................3
1．2 对羟基苯乙酸系列产品的发展前景...................................3
2．实验操作部分.........................................................4
2．1 实验原料与仪器...................................................4
2．1．1 实验原料....................................................4
2．1．2 实验仪器....................................................5
2．2 β一对羟基苯乙醇的合成...........................................5
2．2．1合成路线.....................................................5
2．2．2合成步骤.....................................................6
2．2．2．1对烯丙氧基溴苯的制备....................................6
2．2．2．2对烯丙氧基苯乙醇的制备..................................7
2．2．2．2．1实验准备...........................................7
2．2．2．2．2以无水四氢呋喃作溶剂制备对烯丙氧基苯乙醇...........8
2．2．2．3对羟基苯乙醇的制备......................................10
3．合成工艺实验设计与结果讨论...........................................11
3．1对烯丙氧基溴苯的制备条件..........................................11
3．1．1反应时间对产率的影响........................................11
3．1．2反应温度对产率的影响........................................12
3．1．3丙酮用量对产率的影响........................................12
3．1．4无水碳酸钾用量对产率的影响..................................13
3．1．5对溴苯酚与3一溴丙烯物质量之比对产率的影响..................14
3．1．6正交实验设计................................................14
3．1．7正交实验结果讨论............................................15
3．2合成对烯丙氧基苯乙醇影响因素初探.................................16
3．2．1反应温度对产率的影响.........................................16
3．2．1．1制备格氏试剂过程中反应温度对产率的影响..................16
3．2．1．2滴加环氧乙烷过程中反应温度对产率的影响..................17
3．2．2滴加时间对产率的影响..........................................18
3．2．2．1对烯丙氧基溴苯滴加时间对产率的影响......................18
3．2．2．2环氧乙烷滴加时间对产率的影响............................18
4. 结论................................................................19
附录...................................................................21
附图1 对烯丙氧基溴苯红外图谱.........
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