反应详情

温度

60 °C

Compound 272 (100 mg, 0.37 mmol) was dissolved in dry DMF (1 mL). Sodium hydride, 60% dispersion in oil (16.0 mg, 0.4 mmol) was added and the reaction stirred at 60° C. for 20 minutes. Iodomethane (26.5 μl, 423 μmol) was the added and the reaction stirred at 60° C. for 2 hr. The solution was allowed to cool and added to water (10 mL1) and aqueous K2CO3 (saturated, 2 mL), and extracted with ethyl acetate (2×30 mL), and dichloromethane+10% methanol (2×30 mL1). The combined organics were dried (MgSO4) and evaporated to give an orange solid. Silica gel chromatography (gradient elution hexanes+2.5% TEA/0-70% ethyl acetate+2.5% TEA) afforded compound 273 as a white solid, 64 mg (61%).

1. additionadded
2. stirringthe reaction stirred at 60° C. for 2 hr
3. temperatureto cool
4. extractionextracted with ethyl acetate (2×30 mL), and dichloromethane+10% methanol (2×30 mL1)
5. dry with materialThe combined organics were dried (MgSO4)
6. customevaporated
7. customto give an orange solid
8. washSilica gel chromatography (gradient elution hexanes+2.5% TEA/0-70% ethyl acetate+2.5% TEA)