HRID2416087

反应详情

EQUATION

反应方程式

HRID 2416087 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
36 °C

PROCEDURE

实验过程

A solution of (E)-N-{4-[4-(benzyloxy)-3-chloroanilino]-3-cyano-7-ethoxy-6-quinolinyl}-4-(dimethylamino)-2-butenamide (400 mg, 0.719 mmol) and 1.5 mL of 2N dimethylamine in THF was heated at 36° C. in a sealed tube for 20 hours. After the volatile solvents were stripped off, the residue was treated with 1.5 mL of 2N dimethylamine in THF, and heated again at 36° C. in a sealed tube for 20 hours. After the solvent was removed, the residue was purified by preparatory TLC (developed in ethyl acetate:methanol:triethylamine=10:1:1) to yield 260 mg of the title compound as a yellow solid (yield: 60%), mp 102-104° C.; MS (ES) 601.3 (M+1).

WORKUP

后处理

  1. customAfter the solvent was removed
  2. customthe residue was purified by preparatory TLC (developed in ethyl acetate:methanol:triethylamine=10:1:1)