反应详情

温度

0 °C

A 25% (w/w) solution of sodium methoxide in methanol (2.71 mL, 12.8 mmol, 1 eq) was added to a stirred solution of the crude 3a-Methyl-6-(3-oxo-butyl)-1,2,4,5,9a,9b-hexahydro-3aH-9-oxa-cyclopenta[a]naphthalene-3,7-dione in toluene (200 mL) at 0° C. The resulting mixture was stirred at 0° C. for 0.5 h. The reaction was then quenched with a 10:1 (v/v) of ammonium chloride/potassium bisulfate solution (100 mL). The aqueous layer was extracted with ethyl acetate (2×100 mL), and the combined organic layer was dried with magnesium sulfate. The resulting solution was filtered, evaporated and the residue purified by flash chromatography using 30-50% ethyl acetate in hexane to yield the title compound as a white solid.

1. customThe reaction was then quenched with a 10:1 (v/v) of ammonium chloride/potassium bisulfate solution (100 mL)
2. extractionThe aqueous layer was extracted with ethyl acetate (2×100 mL)
3. dry with materialthe combined organic layer was dried with magnesium sulfate
4. filtrationThe resulting solution was filtered
5. customevaporated
6. customthe residue purified by flash chromatography