反应详情

温度

80 °C

To a mixture of the alcohol from Step C (0.36 g, 0.79 mmol) in anhydrous N,N-dimethylformamide (10 mL) was added sodium hydride (60% dispersion in mineral oil, 0.064 mg, 1.59 mmol) and cuprous iodide (0.015 g, 0.79 mmol) under a nitrogen atmosphere with stirring. After 30 min the suspension was heated at 80° C. for 1 h, cooled and mixed with a saturated aqueous solution of sodium bicarbonate (50 mL) and extracted with ethyl acetate (3×50 mL). The combined extracts were dried over magnesium sulfate, filtered and evaporated to dryness. Chromatography on silica eluting with a gradient of 20% to 30% EtOAc/hexane gave an oil (0.056 g, 19%): LCMS (+APCI) 368 (M+H).

1. temperaturecooled
2. extractionextracted with ethyl acetate (3×50 mL)
3. dry with materialThe combined extracts were dried over magnesium sulfate
4. filtrationfiltered
5. customevaporated to dryness