反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
Sodium hydride (60% in mineral oil, 161 mg, 4.03 mmol) was added to a suspension of 4-chloroaniline (489 mg, 3.83 mmol) in dimethylsulfoxide (10 mL). The mixture was stirred at 130° C. for 5 minutes. 2-Chloro-6-(3,5-dimethyl-pyrazol-1-yl)-pyrazine was added and the resulting mixture was stirred at 130° C. for 30 minutes. Cooling, followed by addition of water gave a brown precipitate. The brown solid was collected by filtration, re-dissolved in ethyl acetate, washed with brine, dried over sodium sulphate, filtrated and evaporated. The crude product was purified by flash chromatography to give (4-chloro-phenyl)-[6-(3,5-dimethyl-pyrazol-1-yl)-pyrazin-2-yl]-amine (318 mg, 55%) as a brown solid.
WORKUP
后处理
- stirringthe resulting mixture was stirred at 130° C. for 30 minutes
- temperatureCooling
- customgave a brown precipitate
- filtrationThe brown solid was collected by filtration
- dissolutionre-dissolved in ethyl acetate
- washwashed with brine
- dry with materialdried over sodium sulphate
- filtrationfiltrated
- customevaporated
- customThe crude product was purified by flash chromatography