HRID2233912

反应详情

EQUATION

反应方程式

HRID 2233912 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of methyl 2-chloro-6-(4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidin-1-yl)pyrimidine-4-carboxylate (Example 6: 380 mg, 0.85 mmol), 2-morpholin-4-ylethanamine (222 mg, 1.70 mmol) and TEA (0.12 ml, 0.85 mmol) in DMF (3 ml) were stirred at 60° C. under nitrogen for 18 hours. The mixture was cooled to room temperature and diluted with EtOAc (75 ml) and water (10 ml). The organic layer was separated, dried over Na2SO4, filtered and concentrated under vacuum. Purification by reversed-phase HPLC (water/acetonitrile gradient, 5-95%) provided 110 mg of the title compound.

WORKUP

后处理

  1. customThe organic layer was separated
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated under vacuum
  5. customPurification by reversed-phase HPLC (water/acetonitrile gradient, 5-95%)