问题：1-cyclopropyl-1,3-butanedione的合成方法
类型：求助 (悬赏分:3分)
提问：kangrui369
等级：▲
版块：有机化学问题(jimuwei,fpcwin1211,netpanda,yjgzfl,Ftian,)
信誉：50%
回复：2
阅读：413
时间：2007-08-09 14:31:58 编辑加入/取消收藏订制/取消短消息举报该贴

哪位知道1-cyclopropyl-1,3-butanedione的合成方法及提纯方法，以及其理化性质？请帮帮忙吧，兄弟在这先谢了。

回复人：afc,★★ (氟化学产品) 时间：2007-08-09 14:37:12 编辑

1楼

To a stirred solution of 8.4 g (0.1 mol) of cyclopropyl methyl ketone in 100 mL of ethyl acetate under nitrogen was added dropwise 39 mL (0.1 mol) of a 21 wt % solution of sodium ethoxide in absolute ethanol. The flask was fitted with a condenser and Dean-Stark trap and was heated. The ethanol was removed by azeotropic distillation. Additional ethyl acetate was added to the flask as needed. After three hours the temperature of the distillate had reached 75.degree. C. and the reaction was allowed to cool and stand overnight. The white solid which precipitated out was collected by filtration and the filtrate was set aside. The solid was dissolved in water and this solution was acidified at 0.degree. C. with 10% aqueous hydrochloric acid. This solution was extracted three times with ethyl ether. The ethyl acetate filtrate was washed with water three times, acidified with 10% aqueous hydrochloric acid, and extracted with ethyl ether. The ether extracts from both extractions were combined, dried over magnesium sulfate, and filtered. Removal of solvents gave 3.5 g of 1-cyclopropyl-1,3-butanedione as an oil. Analysis by GC showed 75% purity. This intermediate was used without further purification.

回复人：kangrui369,▲ () 时间：2007-10-10 15:17:48 编辑	2楼
已经打分了！

得分人：

问题讨论没有结束...

您尚未进入本论坛,登录之后才可以回贴

8msec