反応 #8708

反応方程式

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

収率 68.7%

溶媒

DMSO

water

反応条件

後処理

1. 1
   抽出extracted twice with diethyl ether
2. 2
   その他The precipitate was collected
3. 3
   洗浄washed with water and diethyl ether
4. 4
   その他dried

実験手順

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.

出典