反应详情

To a solution of ketone from Example 25, Step 1 (1.5 g, 3.61 mmol) in dry THF (15 mL) at 0° C. was added a 1M solution of allyl magnesium bromide (4.3 mL, 4.3 mmol). The reaction mixture was stirred for 45 minutes at 0° C., at which point saturated NH4Cl solution (15 mL) was added, and the product was extracted with EtOAc. The organic layer was washed with water and brine, and was then evaporated to dryness. Purification by flash chromatography (gradient of 1:20, 1:10, 1:5 EtOAc/hexane) gave a pale yellow syrup which was triturated with 1:4 ether/hexane to give the title compound as a white solid, m.p.=87°-88° C.

1. additionwas added
2. extractionthe product was extracted with EtOAc
3. washThe organic layer was washed with water and brine
4. customwas then evaporated to dryness
5. customPurification by flash chromatography (gradient of 1:20, 1:10, 1:5 EtOAc/hexane)
6. customgave a pale yellow syrup which
7. customwas triturated with 1:4 ether/hexane