反应详情

2-methyl-1-propenylmagnesium bromide (3 mL, 0.5 M in THF) was added dropwise to a solution of compound 33.1 (1.0 mmol) in THF. The reaction mixture was stirred at room temperature for 1 hr and then quenched with saturated NH4Cl(aq) and the aqueous layer extracted with ethyl acetate twice. The combined organic layers were washed with water and saturated brine, dried over Na2SO4, and concentrated in vacuo. The resulting residue was purified using silica gel column chromatography (hexane/ethyl acetate=2/1) to give compound 33.2 as a white solid (0.93 mmol).

1. customquenched with saturated NH4Cl(aq)
2. extractionthe aqueous layer extracted with ethyl acetate twice
3. washThe combined organic layers were washed with water and saturated brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated in vacuo
6. customThe resulting residue was purified