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594306435

银虫 (小有名气)

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虫号: 716245

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将化合物1溶解在亚磷酸三乙酯，在40℃条件下反应1 h, 冷却，把过量的亚磷酸三乙酯通过减压蒸出。所得到的产品直接溶解在干燥的DMF中，然后加入NaH 和芳香醛，先室温搅拌1 h，再加热到30℃反应1 h，最后加入5mL 5% NaOH溶液，反应过程用TLC监控，待完全反应后，冷却，用1mmol/L HCl酸化，析出的固体经抽滤得固体粗产物x和。粗产物用乙醇重结晶后化合物发生了变化得到了化合物纯品，其余化合物没有变化。

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1楼 2011-04-04 19:42:06

已阅回复此楼关注TA 给TA发消息送TA红花 TA的回帖

charleygan

至尊木虫 (著名写手)

594306435(金币+10, 翻译EPI+1): 太谢谢了 2011-04-06 16:47:53

Compound 1 was dissolved in triethyl phosphite and reacted for an hour at 40 degree C. Then the solution was cooled down, and the excess triethyl phosphite was separated by distillation under reduced pressure. The resulting product was directly dissolved in absolute DMF, then, NaH and aromatic aldehyde were added and stirred for 1 hr at room temperature and another 1 hr at 30 ° C, finally, 5mL 5%NaOH was added into the solution. The whole reaction process was monitored by TLC. After the reaction, the solution was cooled down and an acidification was carried out with 1mmol/L HCl, a solid rough product x was obtained by filtration. The pure product was prepared by recrystallization of compound with ethanol and the remaining compounds kept unchanged.

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