反应详情

温度

40 °C

A mixture of N-tert-butoxycarbonyl-4-(2-bromo-5-methoxybenzal)piperidine (87.7 g, 0.229 mol), 5% rhodium-carbon (25.6 g), ethyl acetate (150 mL) and ethyl alcohol (150 mL) was stirred at 40° C. for 16 hours under a hydrogen atmosphere. The precipitate was filtered and then washed with ethyl acetate, and the filtrate was concentrated to dryness. The residue was diluted with ethyl acetate (800 mL) and washed with a saturated aqueous sodium chloride solution (100 mL). The dilution was dried over anhydrous magnesium sulfate and then concentrated to dryness to obtain 78.7 g (0.205 mol, 89%) of N-tert-butoxycarbonyl-4-(2-bromo-5-methoxybenzyl)piperidine.

1. filtrationThe precipitate was filtered
2. washwashed with ethyl acetate
3. concentrationthe filtrate was concentrated to dryness
4. additionThe residue was diluted with ethyl acetate (800 mL)
5. washwashed with a saturated aqueous sodium chloride solution (100 mL)
6. dry with materialThe dilution was dried over anhydrous magnesium sulfate
7. concentrationconcentrated to dryness