HRID878373

反应详情

EQUATION

反应方程式

HRID 878373 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of N-(4-(2-(benzyloxy)phenyl)-6-methylpyridin-3-yl)-N-methyl-3-(methylsulfonyl)-5-(trifluoromethyl)benzamide (1.63 g, 2.94 mmol) in MeOH (16 mL) and EtOAc (16 mL) was added Pd on carbon (10%, 200 mg, 2.94 mmol) under argon atmosphere. The reaction was evacuated and purged with hydrogen. The reaction was stirred for 5 hours at 1.7 bar under hydrogen atmosphere. The reaction mixture was filtered over dicalite. The filtrate was concentrated under vacuum and the compound was purified by silica gel chromatography on a 50 g column using an MPLC system (CombiFlash Companion, Isco Inc.) eluting with a gradient of n-heptane:EtOAc (100:0 to 0:100). Colorless solid (1.367 g, 100%). MS (ESI): m/z=465.109 [M+H]+.

WORKUP

后处理

  1. customThe reaction was evacuated
  2. custompurged with hydrogen
  3. filtrationThe reaction mixture was filtered over dicalite
  4. concentrationThe filtrate was concentrated under vacuum
  5. customthe compound was purified by silica gel chromatography on a 50 g column
  6. washeluting with a gradient of n-heptane:EtOAc (100:0 to 0:100)