反应详情

To a solution of tert-butyl phosphine (1.40 mL, 11.5 mmol) in THF (40 mL) was added dropwise n-BuLi (11.5 mmol) at −78° C. The resulting yellow solution was allowed to warm to rt and stirred at rt for 1 h. A solution of 40 (2.29 g, 11.5 mmol) in THF (20 mL) was added at −78° C. via cannula. The resulting solution was allowed to warm to rt and stirred at rt for 5 h. After being cooled to 31 78° C. again, n-BuLi (11.5 mmol) was added dropwise. The reaction mixture was warmed to rt and stirred overnight. 2.5 mL H2O2 (30% aq.) was added at 0° C. After being stirred at 0° C. for 1 h, the reaction was quenched with saturated Na2SO3 solution (10 mL) at 0° C. for 1 h. After usual workup, the crude product was purified by recrystallization (CH2Cl2 and hexane) to give 50 as white crystals (2.26 g, 94%).

1. temperatureto warm to rt
2. stirringstirred at rt for 5 h
3. temperatureAfter being cooled to 31 78° C. again
4. temperatureThe reaction mixture was warmed to rt
5. stirringstirred overnight
6. stirringAfter being stirred at 0° C. for 1 h
7. customthe reaction was quenched with saturated Na2SO3 solution (10 mL) at 0° C. for 1 h
8. customAfter usual workup, the crude product was purified by recrystallization (CH2Cl2 and hexane)