反应详情

A solution of i-PrMgCl (9.65 mL, 19.3 mmol) in THF was added dropwise to a solution of compound 1-2 (5.24 g, 19.3 mmol) in dry THF at −5.deg.C. After stirring for 20 min, a solution of BnMgCl (29 mL, 2M, 58 mmol) in THF was added dropwise to the reaction mixture. After completion of addition, the reaction mixture was stirred for 1 h at 0.deg.C, then warmed slowly to room temperature, and stirred for another 1 h. The reaction was quenched with saturated NH4 Cl solution, extracted with ethyl acetate. Separated and collected the organic layer, and the aqueous solution was washed EA for two times. The combined organic layer was washed with brine, dried and concentrated in vacuo to get the crude product, which was purified by silica chromatography to give 5.5 g of ketone 1-3.

1. additionAfter completion of addition
2. stirringthe reaction mixture was stirred for 1 h at 0.deg.C
3. stirringstirred for another 1 h
4. customThe reaction was quenched with saturated NH4 Cl solution
5. extractionextracted with ethyl acetate
6. customSeparated
7. customcollected the organic layer
8. washthe aqueous solution was washed EA for two times
9. washThe combined organic layer was washed with brine
10. customdried
11. concentrationconcentrated in vacuo
12. customto get the crude product, which
13. customwas purified by silica chromatography