反应详情

A solution of dibutyl dicarbonate (25.0 g, 116 mmol) in tetrahydrofuran (40 ml) was added to a solution of 2-(isopropylamino)ethanol (10.0 g, 96.9 mmol) in tetrahydrofuran (60 ml) under ice-cooling. The mixture was stirred at room temperature for 3.5 hours, then a 10% aqueous citric acid solution (500 ml) was added to the reaction mixture, and the whole was extracted with ethyl acetate (500 ml). The organic layer was washed with saturated brine (500 ml) and dehydrated with anhydrous magnesium sulfate. Ethyl acetate was evaporated under reduced pressure, and the obtained oily matter was purified by silica gel column chromatography (mobile phase: hexane/ethyl acetate=1/1) to give 24.0 g (quantitatively) of the target compound.

1. temperaturecooling
2. extractionthe whole was extracted with ethyl acetate (500 ml)
3. washThe organic layer was washed with saturated brine (500 ml)
4. customEthyl acetate was evaporated under reduced pressure
5. customthe obtained oily matter was purified by silica gel column chromatography (mobile phase: hexane/ethyl acetate=1/1)
6. customto give 24.0 g (quantitatively) of the target compound