反应详情

Glucosamine hydrochloride (50 g, 231 mmol) was suspended in anhydrous methanol (500 mL), then 2-acetyl-dimedone sodium salt (47.3 g, 231 mmol) was added. The reaction mixture was stirred at room temperature for 10 minutes, then 2-acetyl-dimedone (21.1 g, 115.9 mmol) was added. The reaction mixture was stirred under reflux for 2.5 hours and monitored by tlc. At the completion of the reaction (TLC: MeCN—H20, 10:2), the reaction mixture was cooled to room temperature and filtered. The filtrate was evaporated and the resulting solid residue was washed on a funnel with ether (3×500 mL) and dried to give crude product (75 g, 94%). No further purification was required for the next reaction.

1. stirringThe reaction mixture was stirred
2. temperatureunder reflux for 2.5 hours
3. temperaturethe reaction mixture was cooled to room temperature
4. filtrationfiltered
5. customThe filtrate was evaporated
6. washthe resulting solid residue was washed on a funnel with ether (3×500 mL)
7. customdried