HRID592415

反应详情

EQUATION

反应方程式

HRID 592415 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 2-(2-((2,5-dichloropyrimidin-4-yl)ethynyl)phenyl)propanamide A29 (1.0 g, 3.1 mmol) in DMF (55 mL) and MeOH (5 mL) was stirred with platinum(II)oxide (0.21 g, 0.94 mmol) under an atmosphere of hydrogen for 120 hours at ambient temperature. The reaction mixture was diluted with EtOAc and filtered through a plug of Celite. The filter cake was washed with EtOAc and the solvents were removed in vacuo to give a crude residue that was purified by silica gel column chromatography (Combiflash Rf, 0-90% EtOAc in cyclohexane), giving the title compound A30 as an off white solid (0.65 g, 64%). LCMS-C: rt 4.98 min; m/z 324 [M+H]+.

WORKUP

后处理

  1. filtrationfiltered through a plug of Celite
  2. washThe filter cake was washed with EtOAc
  3. customthe solvents were removed in vacuo
  4. customto give a crude residue that
  5. customwas purified by silica gel column chromatography (Combiflash Rf, 0-90% EtOAc in cyclohexane)