反应详情

温度

70 °C

Step 2): 1-Diphenylmethylpiperidine-4-carboxamide (1.5 g, 5.1 mmol) was added dropwise to a suspension of LiAlH4 (0.4 g, 10.5 mmol) in THF (30 ml). The mixture was heated at 70° C. for 3 hours and then cooled. To the mixture, water (0.4 ml), 15% NaOH solution (0.4 ml) and water (1.2 ml) were added dropwise in order, and insoluble materials were filtered off. The filtrate was concentrated. The residue was purified by column chromatography on silica gel (10% methanol in dichloromethane) to give 4-aminomethyl-1-diphenylmethylpiperidine (57.0%) as colorless crystals: mp 80° C.

1. temperaturecooled
2. filtrationwere filtered off
3. concentrationThe filtrate was concentrated
4. customThe residue was purified by column chromatography on silica gel (10% methanol in dichloromethane)