反应详情

A mixture of trans-3-bromo-2,2-diethyl-3,4-dihydro-4-hydroxy-2H-1-benzopyran-6-carbonitrile (1.95 g) and potassium carbonate (1.74 g) in N,N-dimethylformamide (8 ml) was stirred overnight at ambient temperature. The reaction mixture was poured into water, extracted with ethyl acetate, and then washed with water and brine successively. The extract was dried over anhydrous magnesium sulfate, treated with active charcoal, and evaporated in vacuo. The residue was purified with silica gel column chromatography using a mixture of methylene chloride and n-hexane (1:2) as an eluent to give 3,4-epoxy-2,2-diethyl-3,4-dihydro-2H-1-benzopyran-6-carbonitrile (1.17 g).

1. extractionextracted with ethyl acetate
2. washwashed with water and brine successively
3. dry with materialThe extract was dried over anhydrous magnesium sulfate
4. additiontreated with active charcoal
5. customevaporated in vacuo
6. customThe residue was purified with silica gel column chromatography
7. additiona mixture of methylene chloride and n-hexane (1:2) as an eluent