HRID334868

反应详情

EQUATION

反应方程式

HRID 334868 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 6-methyl-1-(2,2,2-trifluoroethyl)-5-(2,3,5-trifluorophenyl)pyridin-2(1H)-one (3.73 g, 11.6 mmol) and platinum(IV) oxide (659 mg, 2.90 mmol) in MeOH (200 mL) was shaken on a Parr hydrogenation apparatus under an atmosphere of hydrogen (ca. 45 psi) for 2 h. The reaction mixture was filtered through a pad of Celite®, washing with MeOH, and the filtrate was concentrated in vacuo to give a crude solid. The crude product was purified by silica gel chromatography, eluting with a gradient of hexanes:Et2O—100:0 to 0:100, to give the title compound. MS: m/z=326.0 (M+1).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through a pad of Celite®
  2. washwashing with MeOH
  3. concentrationthe filtrate was concentrated in vacuo
  4. customto give a crude solid
  5. customThe crude product was purified by silica gel chromatography
  6. washeluting with a gradient of hexanes