HRID592493

反应详情

EQUATION

反应方程式

HRID 592493 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of tert-butyl 1-(4-(4-((2-(1-carbamoylcyclopropyl)phenyl)ethynyl)-5-(trifluoromethyl)pyrimidin-2-ylamino)phenyl)ethylcarbamate (0.25 g, 0.44 mmol) in EtOAc (12 mL) and DMF (2.0 mL) was stirred with Pd/C 10% (0.15 g) under an atmosphere of hydrogen for 16 hours at ambient temperature. The reaction mixture was diluted with EtOAc, filtered through a plug of Celite and washed with EtOAc. The solvents were removed in vacuo and the crude residue was purified by silica gel column chromatography (Combiflash Rf 0-100% EtOAc in cyclohexane) to give the title compound 70 as a colourless oil (0.14 g, 56%). LCMS-C: rt 5.88 min; m/z 570 [M+H]+.

WORKUP

后处理

  1. filtrationfiltered through a plug of Celite
  2. washwashed with EtOAc
  3. customThe solvents were removed in vacuo
  4. customthe crude residue was purified by silica gel column chromatography (Combiflash Rf 0-100% EtOAc in cyclohexane)