HRID2066723

反应详情

EQUATION

反应方程式

HRID 2066723 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 1-ethyl-4-(3-fluoro-4-nitro-phenyl)-piperazine (7 g, 27.7 mmol) and Pd (10%) on carbon (0.35 g) in MeOH (140 mL) is stirred for 3 h at RT, under a hydrogen atmosphere. The reaction mixture is filtered through a pad of celite and concentrated. The residue is purified by silica gel column chromatography (DCM/MeOH+1% NH2aq, 95:5) to afford the title compound as a white solid: ESI-MS: 224.1 [MH]+; TLC: Rf=0.54 (DCM/MeOH+1% NH3aq, 95:5).

WORKUP

后处理

  1. filtrationThe reaction mixture is filtered through a pad of celite
  2. concentrationconcentrated
  3. customThe residue is purified by silica gel column chromatography (DCM/MeOH+1% NH2aq, 95:5)