反应详情

温度

-90 °C

To a solution of 11.7 g (32.0 mmol) of 17 in 260 mL of THF, 37 mL (33.6 mmol) of 0.91 M MeLi*LiBr in THF was added dropwise with vigorous stirring for 20 min at −90° C. The reaction mixture was slowly warmed to room temperature and 50 mL of water was added. The organic solvent was evaporated using a rotary evaporator. The crude product was extracted from the residue with 2×100 mL of dichloromethane. The combined extract was dried over Na2SO4 and then evaporated to dryness. This procedure gave 12.0 g (98%) of 18.

1. additionwas added dropwise
2. temperatureThe reaction mixture was slowly warmed to room temperature
3. customThe organic solvent was evaporated
4. customa rotary evaporator
5. extractionThe crude product was extracted from the residue with 2×100 mL of dichloromethane
6. extractionThe combined extract
7. dry with materialwas dried over Na2SO4
8. customevaporated to dryness