反应详情

A suspension of 1-(4-methoxy-benzyl)-4-(5-nitro-pyridin-2-ylmethyl)-piperazine (Step 111.2) (0.635 g, 1.85 mmol) and Raney Nickel (0.150 g) in MeOH/THF (1:1, v/v; 50 mL) was stirred for 24 h at rt, under a hydrogen atmosphere. The mixture was filtered through a pad of celite and the filtrate was concentrated. The residue was purified by silica gel column chromatography (DCM/MeOH/NH3aq, 98:1:1) to afford 439 mg of the title compound as a white solid. Title compound: ESI-MS: 313.3 [M+H]+; tR=1.40 min (System 1); TLC: Rf=0.18 (DCM/MeOH, 9:1).

1. filtrationThe mixture was filtered through a pad of celite
2. concentrationthe filtrate was concentrated
3. customThe residue was purified by silica gel column chromatography (DCM/MeOH/NH3aq, 98:1:1)