HRID243539

反应详情

EQUATION

反应方程式

HRID 243539 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1000 ml of dichloromethane and 100 g of N-[6-chloro-2-(4-cyanophenylamino)pyrimidin-4-yl]benzamide were added to a reaction vessel. To this was added 76.5 g of N-bromosuccinamide and 2.2 g (10M %) of ammonium acetate and stirred for 4 hrs. After completion of the reaction, the pH was adjusted to 10-11 with 5% of aqueous sodium hydroxide solution (10 g in 200 ml water). The reaction mass was filtered and the wet cake was slurried in 1000 ml of hot water at 55-60° C. for 1 hr and filtered. The obtained solid was dried under vacuum (0.5 kg/cm2) at 55-60° C. overnight.

WORKUP

后处理

  1. customAfter completion of the reaction
  2. filtrationThe reaction mass was filtered
  3. waitthe wet cake was slurried in 1000 ml of hot water at 55-60° C. for 1 hr
  4. filtrationfiltered
  5. customThe obtained solid was dried under vacuum (0.5 kg/cm2) at 55-60° C. overnight