反应详情

A solution of 3H-Benzofuran-2-one (4.02 g, 30 mmol) dissolved in THF (15 mL) was added cautiously to a suspension of NaH (95% dry, 1.58 g, 66 mmol) in DMF (60 mL) and THF (30 mL) under a nitrogen atmosphere, at 0° C. The mixture was stirred until gas evolution ceased, then MeI (5.6 mL, 90 mmol) was added slowly to avoid boiling over. After MeI addition was complete the reaction further stirred 1 h at room temperature then quenched by carefully pouring onto a mixture of HCl (1N) and ice. The resulting solution was extracted with ether, washed with brine, dried over MgSO4, and chromatographed on silica eluted with a gradient of 5-50% ethyl acetate/hexanes, yielding 3.16 g (65% yield) of the product.

1. stirringfurther stirred 1 h at room temperature
2. customthen quenched
3. additionby carefully pouring onto a mixture of HCl (1N) and ice
4. extractionThe resulting solution was extracted with ether
5. washwashed with brine
6. dry with materialdried over MgSO4
7. customchromatographed on silica
8. washeluted with a gradient of 5-50% ethyl acetate/hexanes