反应详情

温度

-70 °C

A solution of 2.5M n-BuLi in hexanes (60 ml, 0.15 mol) was added drop-wise to a solution of (4-chloro-2,6-difluorophenyl)trimethylsilane (assumed 0.13 mol) in THF (180 mL) cooled to −70° C. under Ar. After the addition was complete, the mixture was stirred for 1 h before a solution of N-formylmorpholine (20 mL, 0.2 mol) in THF (25 mL) was added dropwise. The reaction was allowed to warm to rt with stirring and then cooled to 0° C. and quenched with H2O. Ether was added, the phases were separated, the aqueous phase was re-extracted with ether and the combined organics washed with brine, dried over MgSO4 and concentrated in vacuo to give the title compound (35 g) as an orange oil which was used without further purification.

1. additionAfter the addition
2. additionwas added dropwise
3. temperatureto warm to rt
4. temperaturecooled to 0° C.
5. customquenched with H2O
6. additionEther was added
7. customthe phases were separated
8. extractionthe aqueous phase was re-extracted with ether
9. washthe combined organics washed with brine
10. dry with materialdried over MgSO4
11. concentrationconcentrated in vacuo