反应详情

温度

0 °C

The title compound from Step B above (2 g, 8.22 mmoles) was dissolved in anhydrous pyridine (10 mL) and the solution was cooled with stirring to 0° C. 4-Toluenesulfonyl chloride (1.88 g, 9.86 mmoles) was added and the mixture was stirred at 0° C. for 2 h. The mixture was evaporated to dryness and the residue was taken up in dichloromethane and washed with saturated aqueous sodium bicarbonate, water, dried (MgSO4), filtered and evaporated to dryness. The product was chromatographed on silica gel using 0.25% methanol in dichloromethane as the eluant to give the title compound (2.53 g, 77%): ESMS: m/z 398.1 (MH+).

1. temperaturethe solution was cooled
2. stirringthe mixture was stirred at 0° C. for 2 h
3. customThe mixture was evaporated to dryness
4. washwashed with saturated aqueous sodium bicarbonate, water
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customevaporated to dryness
8. customThe product was chromatographed on silica gel using 0.25% methanol in dichloromethane as the eluant