HRID2066721
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A suspension of 1-(3-chloro-4-nitro-phenyl)-4-ethyl-piperazine (1 g, 3.7 mmol) and Raney Nickel (0.1 g) in MeOH (20 mL) is stirred for 8 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% NH3aq, 95:5) to afford the title compound as an off-white solid: ESI-MS: 240.1/242.1 [MH]+; tR=0.90 min (system 1), TLC: Rf=0.46 (DCM/MeOH+1% NH3aq, 95:5).
WORKUP
后处理
- filtrationThe reaction mixture is filtered through a pad of celite
- concentrationconcentrated
- customThe residue is purified by silica gel column chromatography (DCM/MeOH+1% NH3aq, 95:5)