反応 #8692

反応方程式

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

収率 21.8%

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
   その他further purified by column chromatography on silica gel eluting with hexane:EA 1:1

実験手順

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.

出典