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baba2846

金虫 (正式写手)

[求助] claisen 酮酯缩合

苯乙酮 甲酸乙酯 碱  生成3-氧代苯丙醛的具体操作流程。
希望有有关实验经验的同学说一下。纯理论的给一篇文献也好。谢谢
perfect is a girl
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li273273

至尊木虫 (职业作家)

暗黑破坏神

【答案】应助回帖

baba2846(金币+5, 博学EPI+1): 2011-11-08 01:21:18
下面是一个claisen 酮酯缩合反应的具体操作过程,你参考下吧
NaH ( 0.225 mol )was added to a dry flask under N2, then THF (200 mL) was added. The reaction mixture was cooled to 0  °C. During the cooling process, 酯( 0.150 mol) was added in one portion, then 酮 ( 0.15mol) was added dropwise over 30 minutes. The mixture was stirred at 0 °C for 1 h, allowed to warm to ambient temperature and was heated to 65 °C for 16 hours. The solvent was removed and diluted with water, and extracted to remove unreacted material. The aqueous phase was acidified with 1N HCl and extracted with DCM. The organic layer was washed with water, brine and dried to yield (11.2 g, 33%)
没有我破坏不了的
2楼2011-11-06 10:39:51
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