反应详情

温度

-10 °C

To a cold (−78° C.) solution of 2,2-dimethyl-4(tol-4-yl)-6-bromo-thiochrom-3-ene (Compound N, 280 mg, 0.81 mmol) in THF (5 mL) was added n-BuLi in hexane (1.6 M solution, 0.66 mL). The mixture was gradually warmed to −10° C. over 25 min. and recooled to −78° C. To this solution was added DMF (80 mg, 1.1 mmol) and stirred at ambient temperature for 5 hours. The reaction was quenched by adding water (10 mL), ethyl acetate (100 mL), and the organic layer was washed with brine (10 mL), dried and the solvent removed by distillation. The crude material was used in the next reaction without further purification.

1. customrecooled to −78° C
2. customThe reaction was quenched
3. additionby adding water (10 mL), ethyl acetate (100 mL)
4. washthe organic layer was washed with brine (10 mL)
5. customdried
6. customthe solvent removed by distillation
7. customThe crude material was used in the next reaction without further purification