反应详情

温度

70 °C

The compound of Example 181 (0.4 g, 0.757 mmol) was added to aqueous 6 N HCl (10 ml) at 0° C. and the mixture was stirred at 70° C. for 3 h. The mixture was quenched with saturated aqueous sodium bicarbonate solution and extracted with ethyl acetate (3×50 ml). The combined organic layer was washed with water, brine and dried over sodium sulphate and the residue was purified by column chromatography (60-120 silica gel, 10% methanol in DCM) to give the product in 30% yield (0.11 g). LC-MS (ESI): Calculated mass: 486.52; Observed mass: 487.3 [M+H]+ (rt: 0.22 min).

1. customThe mixture was quenched with saturated aqueous sodium bicarbonate solution
2. extractionextracted with ethyl acetate (3×50 ml)
3. washThe combined organic layer was washed with water, brine
4. dry with materialdried over sodium sulphate
5. customthe residue was purified by column chromatography (60-120 silica gel, 10% methanol in DCM)
6. customto give the product in 30% yield (0.11 g)
7. custom487.3 [M+H]+ (rt: 0.22 min)