반응 #8708

반응 방정식

4,6-dichloro-5-(4-chlorophenyl)pyrimidine

2-thiophen-2-yl-ethanesulfonic acid amide potassium salt

Hunig's base

→

2-thiophen-2-yl-ethanesulfonic acid [6-chloro-5-(4-chloro-phenyl)-pyrimidin-4-yl]-amide

수율 68.7%

용매

DMSO

water

반응 조건

후처리

1. 1
   추출extracted twice with diethyl ether
2. 2
   기타The precipitate was collected
3. 3
   세척washed with water and diethyl ether
4. 4
   기타dried

실험 절차

A solution of 4,6-dichloro-5-(4-chlorophenyl)pyrimidine (848 mg), 2-thiophen-2-yl-ethanesulfonic acid amide potassium salt (1.5 g, Referential Example 14) and Hunig's base (1 ml) in DMSO (20 ml) was stirred at rt for 24 h before it was diluted with water (200 ml) and extracted twice with diethyl ether. The aqueous layer was acidified with acetic acid. The precipitate was collected, washed with water and diethyl ether and dried to give 2-thiophen-2-yl-ethanesulfonic acid [6-chloro-5-(4-chloro-phenyl)-pyrimidin-4-yl]-amide (930 mg) as a beige powder. LC-MS: tR=5.01 min, [M+1]+=413.49, [M−1]−=411.93.

출처