HRID733732

反应详情

EQUATION

反应方程式

HRID 733732 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 4-chloro-1-methyl-7-(4-morpholinylcarbonyl)-1H-pyrrolo[3,2-c]pyridine (100 mg), 2-chloro-4-cyanoaniline (60 mg), cesium carbonate (168 mg), tris(dibenzylideneacetone)dipalladium (0) (15 mg) and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (10 mg) in 1,4-dioxan (2 ml) was heated to 100° C. under nitrogen for 2 h. Added tris(dibenzylideneacetone)dipalladium (0) (15 mg) and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (10 mg) and continued heating at 100° C. under nitrogen over night. Added tris(dibenzylideneacetone)dipalladium (0) (15 mg) and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (10 mg) and continued heating at 100° C. under nitrogen over night. The reaction mixture was diluted with dichloromethane and washed with water then dried (MgSO4), filtered and evaporated. Purified by trituration with 1:1 methanol:DMSO washing the filtered solid with methanol. Salt formation was as described in Example 101 to afford the title compound as a pale yellow solid (27 mg).

WORKUP

后处理

  1. washwashed with water
  2. dry with materialthen dried (MgSO4)
  3. filtrationfiltered
  4. customevaporated
  5. customPurified by trituration with 1:1 methanol