HRID369869

反应详情

EQUATION

反应方程式

HRID 369869 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under a N2 atmosphere, 97.6 mg (0.338 mmol) of 6-carboxy-4-(3-chloro-anilino)-7H-pyrrolo[2,3-d]pyrimidine are introduced into 7 ml of DMF, and 119 mg (0.40 mmol) of TPTU and a solution of 164 mg (33% in ethanol; 1.2 mmol) of dimethylamine in 1 ml of DMF are added thereto. After 2 hours, a further 30 mg of TPTU is added to the reaction solution, which is then stirred at RT for 2 days, then poured into 30 ml of ice-water, stirred, filtered and washed with water to yield the title compound; HPLC: tRet (Grad20)=9.5; TLC-Rf =0.38 (CH2Cl2 /methanol [10:1]); FAB-MS: (M+H)+ =316.

WORKUP

后处理

  1. stirringstirred
  2. filtrationfiltered
  3. washwashed with water