HRID369867

反应详情

EQUATION

反应方程式

HRID 369867 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 25 mg (0.6 mmol) of LiOH.H2O in 0.4 ml of H2O is added dropwise to a suspension of 95 mg (0.30 mmol) of 4-(3-chloro-anilino)-6-ethoxycarbonyl-7H-pyrrolo[2,3-d]pyrimidine in 0.7 ml of methanol. The reaction mixture is heated at boiling for 4.5 hours, then cooled in an ice-bath and acidified with 0.6 ml of 1 N HCl solution. Filtering and washing with water yield the title compound; HPLC: tRet (Grad20)=8.7; FAB-MS: (M+H)+ =289.

WORKUP

后处理

  1. temperatureThe reaction mixture is heated
  2. temperaturecooled in an ice-bath
  3. filtrationFiltering
  4. washwashing with water