反应 #40367

反应方程式

water

2,5-dichloro-N-ethyl-N-methylpyrimidin-4-amine

4-nitro-2,5-dimethylphenol

potassium carbonate

→

5-chloro-2-(2,5-dimethyl-4-nitrophenoxy)-N-ethyl-N-methylpyrimidin-4-amine

溶剂

DMF

反应条件

后处理

1. 1
   萃取was extracted twice with 50 ml dichloromethane
2. 2
   洗涤The combined organic layers were washed with aqueous solution of sodium hydroxide
3. 3
   干燥The organic layer was dried over magnesium sulfate
4. 4
   浓缩concentrated in vacuo and column chromatography (dichloromethane)
5. 5
   其他yielded 8.3 g (47%) with a purity of 76%

实验过程

A solution of 16.8 g (40 mmol) 2,5-dichloro-N-ethyl-N-methylpyrimidin-4-amine, 7.35 g 4-nitro-2,5-dimethylphenol (44 mmol) and 8.29 g potassium carbonate (60 mmol) in 70 ml DMF were stirred for 20 hrs at 100° C. After adding the mixture to 150 ml water the resulting suspension was extracted twice with 50 ml dichloromethane. The combined organic layers were washed with aqueous solution of sodium hydroxide. The organic layer was dried over magnesium sulfate, concentrated in vacuo and column chromatography (dichloromethane) yielded 8.3 g (47%) with a purity of 76%; log P (pH=2.3)=4.07.

来源