反应详情

温度

4 °C

15 g of 1 was added in portions to 200 ml of chilled (4°-5° C.), stirred 90% nitric acid, and the mixture was stirred at 4° C. for 30 minutes. The resulting mixture was poured into ice water and the resulting solid was filtered. The filter cake was washed with water and purified by silica gel column chromatography, using as eluent a 66:30:4 (v:v:v) mixture of hexane, ethyl acetate and tetrahydrofuran, to give 2, as an amber glassy solid.

1. temperatureof chilled (4°-5° C.)
2. filtrationthe resulting solid was filtered
3. washThe filter cake was washed with water
4. custompurified by silica gel column chromatography
5. additiona 66:30:4 (v:v:v) mixture of hexane, ethyl acetate and tetrahydrofuran
6. customto give 2