反应 #8692

反应方程式

4,6-dichloro-2-(4-pyridyl)-5-(p-tolyl)-pyrimidine

2-phenyl-ethanesulfonic acid amide potassium salt

Hunig's base

→

2-phenyl-ethanesulfonic acid (6-chloro-2-pyridin-4-yl-5-p-tolyl-pyrimidin-4-yl)-amide

收率 21.8%

溶剂

DMSO

water

反应条件

后处理

1. 1
   萃取extracted twice with diethyl ether
2. 2
   其他The precipitate was collected
3. 3
   其他further purified by column chromatography on silica gel eluting with hexane:EA 1:1

实验过程

A solution of 4,6-dichloro-2-(4-pyridyl)-5-(p-tolyl)-pyrimidine (1.5 g), 2-phenyl-ethanesulfonic acid amide potassium salt (1.44 g, Referential Example 1e) and Hunig's base (1 ml) in DMSO (20 ml) was stirred at rt for 24 h before it was diluted with water (150 ml) and extracted twice with diethyl ether. The aqueous layer was acidified with acetic acid. The precipitate was collected, and further purified by column chromatography on silica gel eluting with hexane:EA 1:1 to give 2-phenyl-ethanesulfonic acid (6-chloro-2-pyridin-4-yl-5-p-tolyl-pyrimidin-4-yl)-amide (480 mg) as a foam. LC-MS: tR=5.08 min, [M+1]+=465.13, [M−1]−=462.96.

来源