تفاعل #8692

معادلة التفاعل

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

المردود 21.8%

المذيبات

DMSO

water

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted twice with diethyl ether
2. 2
   أخرىThe precipitate was collected
3. 3
   أخرىfurther purified by column chromatography on silica gel eluting with hexane:EA 1:1

الإجراء التجريبي

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.

المصدر