反应详情

To saccharin (5.0 g, 0.0273 mol) in DMF (10 mL) was added Nail (1.15 g, 60% in oil, 0.0288 mol) with ice bath cooling. After stirring for 10 minutes. a solution of 3,4-methylenedioxybenzyl chloride in methylene chloride, 50% by weight, (10 g, 0.0293 mol) was added and the mixture stirred for 16 hours. The mixture was diluted with ethyl acetate (200 mL) containing 10% methylene chloride and washed with IN HCl (2×100 mL). The organic phase was washed with brine and dried over MgSO4. The mixture was concentrated until crystals were apparent. After standing for 16 hours the product was collected by filtration (4.2 g, 49%);

1. temperaturecooling
2. stirringthe mixture stirred for 16 hours
3. washwashed with IN HCl (2×100 mL)
4. washThe organic phase was washed with brine
5. dry with materialdried over MgSO4
6. concentrationThe mixture was concentrated until crystals
7. waitAfter standing for 16 hours
8. filtrationthe product was collected by filtration (4.2 g, 49%)