反应详情

Sodium bicarbonate (8.81 g, 0.105 mol) was added to a solution of 15.0 g (0.075 mol) of 3,3-dimethyl-1,5-dioxaspiro<5.5>undecan-9-ol in 150 ml of acetonitrile. The reaction mixture was charged with 15.0 g of silica gel (MCB 60-200 mesh) and 15.0 g of calcium hypochlorite in sequence. The reaction mixture was stirred at a temperature in the range of 24° C. to 28° C. for about 18 hours and then warmed to 29° C. to 30° C. for 4 hours. The mixture was filtered and evaporated under vacuum. The residue was combined with 135 ml of toluene and 50 ml of water, and the resulting mixture was stirred for 45 minutes. The organic phase was separated, washed with 50 ml of a saturated sodium chloride solution and dried over 10.0 g of anhydrous sodium sulfate. A gas chromatograph of the sample showed 93.6% pure product. The organic phase was concentrated under vacuum to afford 13.97 g of 3,3-dimethyl-1,5-dioxaspiro<5.5>undecan-9-one.

1. temperaturewarmed to 29° C. to 30° C. for 4 hours
2. filtrationThe mixture was filtered
3. customevaporated under vacuum
4. stirringthe resulting mixture was stirred for 45 minutes
5. customThe organic phase was separated
6. washwashed with 50 ml of a saturated sodium chloride solution
7. dry with materialdried over 10.0 g of anhydrous sodium sulfate
8. concentrationThe organic phase was concentrated under vacuum