反应 #40361

反应方程式

4-(2-chloro-pyrimidin-4-yloxy)-2,5-dimethyl-phenylamine

N-methylaniline

ethyl acetate

→

[4-(4-Amino-2,5-dimethyl-phenoxy)-pyrimidin-2-yl]-methyl-phenyl-amine

溶剂

hydrochloric acid

反应条件

后处理

1. 1
   workup.ADDITIONwas added
2. 2
   其他the organic layer was separated
3. 3
   过滤the formed precipitate was filtered by suction
4. 4
   洗涤washed with hexane
5. 5
   其他After separation the organic layer
6. 6
   浓缩was concentrated in vacuo and column chromatography (dichloromethane)
7. 7
   其他yielded 380 mg (11%) with a purity of 89% log P (pH=2.3)=1.72

实验过程

A solution of 2.50 g (10 mmol) 4-(2-chloro-pyrimidin-4-yloxy)-2,5-dimethyl-phenylamine and 2.14 g N-methylaniline (20 mmol) in 50 ml hydrochloric acid were stirred for 20 h at 80° C. After cooling down to ambient temperature 50 ml ethyl acetate was added and the organic layer was separated. The water layer was brought to pH 8 with sodium carbonate and the formed precipitate was filtered by suction and washed with hexane. After separation the organic layer was concentrated in vacuo and column chromatography (dichloromethane) yielded 380 mg (11%) with a purity of 89% log P (pH=2.3)=1.72.

来源