反应详情

Potassium tert-butoxide (6.4 g) was added to a solution of dimethyl isophthalate (10.0 g) in acetonitrile (90 ml) at ambient temperature and the mixture was stirred for 1 hour at 60°-64° C. The reaction mixture was added to a solution of conc. hydrochloric acid (4.7 ml) in water (150 ml) and extracted with ethyl acetate. The extract layer was washed with water and dried over magnesium sulfate. Evaporation of the solvent gave a residue, which was purified by column chromatography on silica gel eluting with chloroform. The eluted fractions containing the desired product were collected and evaporated in vacuo to give methyl 3-(cyanoacetyl)benzoate (4.72 g).

1. extractionextracted with ethyl acetate
2. washThe extract layer was washed with water
3. dry with materialdried over magnesium sulfate
4. customEvaporation of the solvent
5. customgave a residue, which
6. customwas purified by column chromatography on silica gel eluting with chloroform
7. additionThe eluted fractions containing the desired product
8. customwere collected
9. customevaporated in vacuo