HRID1864148

反应详情

EQUATION

反应方程式

HRID 1864148 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stream of dry hydrogen chloride was passed through a solution of 1-chloro-N′-[4-cyano-2-(4-methanesulfonyl-phenyl)-2H-pyrazol-3-yl]-N,N-dimethyl-formamidine (0.600 g, 1.70 mmol) in 1,2-dichloroethane (20 mL) for 1 h. The solution was stirred at rt for 3 days. The solvent was removed under reduced pressure and the crude washed several times with dichloromethane. [4-Chloro-1-(4-methanesulfonyl-phenyl)-1H-pyrazolo[3,4-d]pyrimidin-6-yl]-dimethyl-amine recrystalized in dichloromethane and it was retrieved by filtration as an off-white solid (0.4 g, 67%). Exact mass calculated for C14H14ClN5O2S 351.06, found 352.20 (MH+, 100%).

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. washthe crude washed several times with dichloromethane
  3. custom[4-Chloro-1-(4-methanesulfonyl-phenyl)-1H-pyrazolo[3,4-d]pyrimidin-6-yl]-dimethyl-amine recrystalized in dichloromethane
  4. filtrationit was retrieved by filtration as an off-white solid (0.4 g, 67%)