反应详情

To a solution of phosphonium bromide (780 mg) (Step 4) in tetrahydrofuran (THF) (8 mL) at -78° was added dropwise 1 eq. of n-BuLi in hexane. The solution was stirred at -78° for 15 min. Then (545 mg) of the aldehyde (Step 1) in THF (4 mL) was added dropwise and the reaction mixture was stirred at -78° for 1 hour. The reaction mixture was poured into pH 7 buffer, extracted with ethyl acetate, dried and evaporated. The residue was chromatographed on a column of SiO2 using 10:1 toluene/ethyl acetate to afford the title compound, m.p. 66°-67° C.

1. stirringthe reaction mixture was stirred at -78° for 1 hour
2. additionThe reaction mixture was poured into pH 7 buffer
3. extractionextracted with ethyl acetate
4. customdried
5. customevaporated
6. customThe residue was chromatographed on a column of SiO2 using 10:1 toluene/ethyl acetate