反应详情

To a cold (−78° C.) solution of 2-methylthiophene (820 mg, 8.3 mmol) in THF (16 mL) was added n-BuLi in hexane (1.6M, 4.4 mL, 8.5 mmol). The mixture was warmed to ambient temperature and stirred for 15 minutes. This solution was added to a flask containing cold (−78° C.) solution of 2,2-dimethyl-6-bromo-chroman-4-one (1.08 g, 4.2 mmol) in THF (4 mL). The mixture was stirred and allowed to gradually warm to ambient temperature over 8 hours, and then stirred for an additional 4 hours at ambient temperature. The mixture was diluted with ethyl acetate (200 mL), washed with 10% HCl, brine (20 mL), dried and the solvent was removed by evaporation. The product was purified by chromatography on a silica gel column to afford the title compound as a colorless oil.

1. additionThis solution was added to a flask
2. stirringThe mixture was stirred
3. temperatureto gradually warm to ambient temperature over 8 hours
4. stirringstirred for an additional 4 hours at ambient temperature
5. washwashed with 10% HCl, brine (20 mL)
6. customdried
7. customthe solvent was removed by evaporation
8. customThe product was purified by chromatography on a silica gel column