HRID2233936

反应详情

EQUATION

反应方程式

HRID 2233936 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2,4-dichloro-6-methoxy-1,3,5-triazine (commercially available) (0.05 g, 0.32 mmol) in DMF (0.5 ml) was added to a solution of 3,4-dichloro-5-methyl-N-piperidin-4-yl-1H-pyrrole-2-carboxamide hydrochloride (Intermediate 1, 0.1 g, 0.32 mmol) and TEA (0.06 g, 0.64 mmol) in DMF (1.5 ml). The resultant mixture was stirred for 1 h at room temperature, then was diluted with water and extracted with EtOAc. During the aqueous workup, some of the product precipitated and was collected by suction filtration. The organic extract was dried over magnesium sulphate, filtered and concentrated to give the desired product with small amount of impurities.

WORKUP

后处理

  1. extractionextracted with EtOAc
  2. customDuring the aqueous workup, some of the product precipitated
  3. filtrationwas collected by suction filtration
  4. extractionThe organic extract
  5. dry with materialwas dried over magnesium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated