HRID2173716

反应详情

EQUATION

反应方程式

HRID 2173716 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture comprising 3-amino-6-bromo-5-trifluoromethyl-pyridine-2-carboxylic acid (Intermediate 3) (0.10 g, 0.351 mmol), 1H-pyrazolo[3,4-b]pyrazin-3-amine (0.047 g, 0.702 mmol), HATU (0.133 g, 0.351 mmol) and N-methylmorpholine (0.069 ml, 0.702 mmol) in DMF (5 ml) was stirred at 75° C. for 90 minutes. After cooling to RT, the mixture was diluted with water (30 ml) and the resulting orange precipitate was filtered under vacuum and washed with water. Purification of the resulting solid by chromatography on silica eluting with iso-hexane:EtOAc (gradient of 0 to 100% EtOAc) to afforded the title compound as an orange solid.

WORKUP

后处理

  1. filtrationthe resulting orange precipitate was filtered under vacuum
  2. washwashed with water
  3. customPurification of the resulting solid by chromatography on silica eluting with iso-hexane