反应详情

温度

-78 °C

Compound 12 (470 mg, 945 μmol) was dissolved in freshly distilled THF (5 mL) under nitrogen atmosphere and cooled to −78° C. n-butyllithium 1.6M in hexane solution (886 μL, 1.42 mmol) was then added and the mixture stirred 30 min at −78° C. Tributyltin chloride (462 mg, 1.42 mmol) in solution in THF (2 mL) was added and the mixture let to warm to room temperature overnight. A 0.1M ammonium chloride solution (5 mL) was added to the reactionnal mixture. The organic layer was isolated and the aqueous layer was extracted with dichloromethane (2×5 mL). The organic layers were combined and dried over sodium sulfate. After solvent evaporation under reduced pressure, the residue was purified over silica gel with heptane/acetone (98/2) as eluant to give 524 mg (794 μmol, 84% yield) of a yellowish oil.

1. additionwas then added
2. temperatureto warm to room temperature overnight
3. customThe organic layer was isolated
4. extractionthe aqueous layer was extracted with dichloromethane (2×5 mL)
5. dry with materialdried over sodium sulfate
6. customAfter solvent evaporation under reduced pressure
7. customthe residue was purified over silica gel with heptane/acetone (98/2) as eluant