问题：求助合成文献资料
类型：求助 (悬赏分:10分)
提问：bugaode
等级：▲
版块：有机化学问题(jimuwei,fpcwin1211,netpanda,yjgzfl,Ftian,)
信誉：29%
回复：3
阅读：632
时间：2011-05-14 15:34:57 编辑加入/取消收藏订制/取消短消息举报该贴

求助：由环丙基甲基酮(CAS：765-43-5)和乙酸乙酯合成1-环丙基-1，3-丁二酮（CAS：21573-10-4）的文献资料。

回复人：tangyyer,★★★★★ (有空来逛逛my blog: http://tangyyer.blog.hexun.com) 时间：2011-05-16 16:06:28 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 45 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° C. and the
reaction 50 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° C. with 10% aqueous hydrochloric acid. This solution
was extracted 55 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. 60 Removal of solvents gave 3.5 g of l-cyclopropyl-
1,3butanedione as an oil. Analysis by GC showed 75% purity. This
intermediate was used without further purification.

回复人：bugaode,▲ (初来乍到,请多关照.) 时间：2011-05-16 19:03:09 编辑	2楼
这个过程要用到催化剂吗？

回复人：bugaode,▲ (初来乍到,请多关照.) 时间：2011-05-17 17:14:38 编辑	3楼
顶下。

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