反应 #80976

反应方程式

1,3-dichloroacetone

N,N-dimethylthiourea

MgSO4

→

desired compound

收率 70.0%

4-(Chloromethyl)-2-(dimethylamino)thiazole

收率 70.0%

溶剂

acetone

acetone

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度to reflux
3. 3
   温度The resulting mixture was heated
4. 4
   温度at reflux for 1.5 h
5. 5
   温度to cool
6. 6
   过滤filtered
7. 7
   浓缩concentrated in vacuo
8. 8
   其他The residue was purified by silica gel chromatography

实验过程

A mixture of 15 g (144 mmol) of N,N-dimethylthiourea and excess MgSO4 in 350 ml of acetone was heated to reflux and treated dropwise with a solution of 18.3 g (144 mmol) of 1,3-dichloroacetone in 35 ml of acetone. The resulting mixture was heated at reflux for 1.5 h, allowed to cool, filtered, and concentrated in vacuo. The residue was purified by silica gel chromatography using 20% ethyl acetate in hexane to provide 14.0 g (70%) of the desired compound.

来源