反应详情

A benzene solution (120 ml) of 2-cyanobenzaldehyde (30.97 g), methyl 4,4-dimethoxyacetoacetate (46.14 g), acetic acid (2.3 g) and piperidine (2.4 g) was refluxed under heating for 8 hours. After addition of benzene (80 ml) and washing with water, the solution was treated with an activated charcoal. The evaporated residue was chromatographed on silica gel (500 g) with methylene chloride as an eluent. The fractions containing a desired compound were collected and evaporated to give methyl 2-(2-cyanobenzylidene)-4,4-dimethoxyacetoacetate (25.16 g).

1. temperatureunder heating for 8 hours
2. washwashing with water
3. additionthe solution was treated with an activated charcoal
4. customThe evaporated residue was chromatographed on silica gel (500 g) with methylene chloride as an eluent
5. additionThe fractions containing a desired compound
6. customwere collected
7. customevaporated