反应详情

温度

60 °C

The compound (239 mg, 0.57 mmol) obtained in Example 94a was dissolved in methanol (15 mL), paraformaldehyde (179 mg, 5.67 mmol) and 10% palladium-carbon (48 mg, 20% by weight) were added, and the mixture was stirred at 60° C. under a hydrogen atmosphere for 18 hours. After the reaction was completed, the reaction mixture was filtered through celite, the filtrate was washed with methanol, and the solvent was evaporated under reduced pressure. The residue was purified by NH silica gel column chromatography (hexane:ethyl acetate, 10:1, v/v) to give the title compound (172 mg; yield, 70%) as a pale pink oily substance.

1. filtrationthe reaction mixture was filtered through celite
2. washthe filtrate was washed with methanol
3. customthe solvent was evaporated under reduced pressure
4. customThe residue was purified by NH silica gel column chromatography (hexane