HRID2233964

反应详情

EQUATION

反应方程式

HRID 2233964 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

4-Bromo-5-methyl-N-piperidin-4-yl-1H-pyrrole-2-carboxamide hydrochloride (intermediate 57, 0.41 g, 1.27 mmol), sodium bicarbonate (0.42 g, 1.78 mmol) and ethyl 2-bromo-1,3-thiazole-4-carboxylate (0.30 g, 1.27 mmol) were combined in DMF (5 ml) under nitrogen and heated at 50° C. for 18 h. The mixture was cooled to room temperature and diluted with EtOAc (75 ml) and water (10 ml). The organic layer was separated, dried over sodium sulphate, filtered and concentrated under vacuum. Purification by flash chromatography (MeOH/DCM, 10%) provided 275 mg of the title compound.

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. customThe organic layer was separated
  3. dry with materialdried over sodium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated under vacuum
  6. customPurification by flash chromatography (MeOH/DCM, 10%)