反应详情

温度

50 °C

A mixture of 393C (0.84 g, 2 mmol) and K2CO3 (1.0 g, 7.25 mmol) in acetone (5 ml) was heated at 50° C. for 30 min, then cooled to rt. Dimethyl sulfate (0.29 ml, 3.0 mmol) was added, the resulting mixture was heated at 40° C. until starting material consumed, quenched with brine and extracted with EtOAc. The organic layer was dried and concentrated, the residue was purified by silica gel flash column chromatography to afford 393D (0.58 g, 74% for 3 steps from 393B) (0%-5% EtOAc—CH2Cl2).

1. temperaturecooled to rt
2. temperaturethe resulting mixture was heated at 40° C.
3. customconsumed
4. customquenched with brine
5. extractionextracted with EtOAc
6. customThe organic layer was dried
7. concentrationconcentrated
8. customthe residue was purified by silica gel flash column chromatography