反应详情

A solution of fluorene (20.0 g; 120 mmol) in THF (200 mL) was cooled to -40° C. and treated with 48 mL of a 2.5M solution of n-butyllithium in hexanes (120 mmol). After stirring for 15 minutes, a solution of ethylene sulfide (6.5 mL; 109 mmol) in 30 mL of THF was added, and the resulting mixture was stirred at -40° C. for 30 minutes and room temperature for 2 hours. The reaction was quenched by the addition of saturated ammonium chloride, the layers were separated, and the organic phase was washed with 10% HCl, dried and concentrated. The crude product was purified on a flash column, eluting with hexane, to provide 16.8 g (62%) of the product as an oil that recrystallized from hexane as a white solid, mp 38°-40° C.

1. stirringthe resulting mixture was stirred at -40° C. for 30 minutes and room temperature for 2 hours
2. customThe reaction was quenched by the addition of saturated ammonium chloride
3. customthe layers were separated
4. washthe organic phase was washed with 10% HCl
5. customdried
6. concentrationconcentrated
7. customThe crude product was purified on a flash column
8. washeluting with hexane