反应详情

A mixture of magnesium turnings (0.31 g, 13.1 mmol), 2-chloro-4-bromoanisole (3.00 g, 13.5 mmol), 4-tert-butyldimethysilyloxy-2-(3,4,5-trimethoxy-phenyl)-cyclopent-2-en-1-one (2.58 g, 6.84 mmol) and dry tetrahydrofuran (35 ml) under nitrogen was stirred at room temperature for 4 h. Reaction was then quenched with dil hydrochloric acid (30 ml), tetrahydrofuran was removed under reduced pressure and the residual reaction mixture was extracted with ethyl acetate (3×35 ml), washed with water (2×20 ml) and dried over sodium sulfate. Concentration and purification by column chromatography over silica gel (eluent-6% acetone in pet ether) afforded the alcohol of the formula (4A)

1. customReaction
2. customwas then quenched with dil hydrochloric acid (30 ml), tetrahydrofuran
3. customwas removed under reduced pressure
4. customthe residual reaction mixture
5. extractionwas extracted with ethyl acetate (3×35 ml)
6. washwashed with water (2×20 ml)
7. dry with materialdried over sodium sulfate
8. concentrationConcentration and purification by column chromatography over silica gel (eluent-6% acetone in pet ether)