HRID906512

反应详情

EQUATION

反应方程式

HRID 906512 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 5-acetyl-2-acetylamino-4-trifluoromethyl-benzoic acid methyl ester (4 g, 13.2 mmol) in THF (40 mL) was hydrogenated at r.t. for 2 h over Pd—C (10%, 250 mg). The reaction mixture was filtered on a sintered funnel The filtrate was concentrated in vacuo. The residue was purified by column chromatography (silica gel, 2:1 hexanes/EtOAc) to give the title product (3.66 g, 91% yield) as colorless crystals. m.p.: 120-123° C., ESI-MS: m/z 306 [M+H]+.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered on a sintered funnel The filtrate
  2. concentrationwas concentrated in vacuo
  3. customThe residue was purified by column chromatography (silica gel, 2:1 hexanes/EtOAc)