HRID592483

反应详情

EQUATION

反应方程式

HRID 592483 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A mixture of 1-(2-((2-((1-methyl-1H-pyrazol-4-yl)amino)-5-(trifluoromethyl)pyrimidin-4-yl)ethynyl)phenyl)cyclopropanecarboxamide A75 (0.120 g, 0.281 mmol) and 10% Pd/C (0.135 g) in DMF (3 mL), EtOAc (5 mL) and Et3N (0.5 mL) was stirred under a hydrogen atmosphere for 16 hours. The mixture was filtered through Celite and concentrated under reduced pressure before purification by silica gel column chromatography (0-15% MeOH in EtOAc). The product was triturated with Et2O and the resulting precipitate was collected to give the title compound 65 (0.090 g, 74%). LCMS-D: rt 3.316 min; m/z 431.2 [M+H]+.

WORKUP

后处理

  1. filtrationThe mixture was filtered through Celite
  2. concentrationconcentrated under reduced pressure before purification by silica gel column chromatography (0-15% MeOH in EtOAc)
  3. customThe product was triturated with Et2O
  4. customthe resulting precipitate was collected