反应详情

To a solution of ethyl 4-(4-aminophenyl)-4-methylpiperidine-1-carboxylate (444 mg, 1.692 mmol) in THF (10 mL) was added solid LAH (321 mg, 8.46 mmol) portion-wise. The formation of bubbles were observed during addition. The reaction mixture was stirred at room temperature for 20 min. The reaction mixture was diluted with methylene chloride and 15 mL of 1N NaOH was added slowly to destroy excess LAH. The resulting mixture was separated by separatory funnel. The organic layer was washed with water and concentrated. The residue was purified by MPLC (ISCO, 6% ammonia/MeOH/CH2Cl2, 40 g silica gel column) to give 267 mg colorless oil. (M+H)+=205.18.

1. additionThe formation of bubbles were observed during addition
2. additionwas added slowly
3. customto destroy excess LAH
4. customThe resulting mixture was separated by separatory funnel
5. washThe organic layer was washed with water
6. concentrationconcentrated
7. customThe residue was purified by MPLC (ISCO, 6% ammonia/MeOH/CH2Cl2, 40 g silica gel column)