反应详情

A mixture of 2 g of compound 1 and 1 eq sodium ethanolate in 30 ml of dimethylformamide was added to a solution of 2 g of ω-bromo-2-methoxyacetophenone in dimethylformamide. After 30 min small portions of additional ω-bromo-2-methoxyacetophenone (total 5 gram) and sodium ethanolate were added during 2 hours. Subsequently the reaction mixture was evaporated and the residue partitioned between water and ethyl acetate. The organic layer was dried over magnesium sulfate and evaporated. The residue was purified by chromatography (dichloromethane). Crystallized from methanol. M.p. 93°-96° C.

1. customSubsequently the reaction mixture was evaporated
2. customthe residue partitioned between water and ethyl acetate
3. dry with materialThe organic layer was dried over magnesium sulfate
4. customevaporated
5. customThe residue was purified by chromatography (dichloromethane)
6. customCrystallized from methanol