反应详情

To a rapidly stirred solution of 8.33 g potassium carbonate 1.5 hydrate in 330 ml water was added 18.5 g of the nitrophenyl ketone. 2.5 g of potassium carbonate was added to make a clear solution. A solution of 2.36 g sodium borohydride in 50 ml water was added over 5 min. The mixture was heated to 45° for one hour, cooled to room temperature over 2 hours, and shaken with 200 ml ether. The layers were separated and the water layer stirred as a solution of 8% aqueous HCl was added until the solution was a pH of 2-3. An orange solid was collected by filtration, blended in ice water, filtered, washed with water and vacuum oven dried at 60° C. to yield 18 g, 95% yield.

1. temperatureThe mixture was heated to 45° for one hour
2. customThe layers were separated
3. additionwas added until the solution
4. filtrationAn orange solid was collected by filtration
5. filtrationfiltered
6. washwashed with water and vacuum oven
7. customdried at 60° C.
8. customto yield 18 g, 95% yield