反应详情

A mixture of 1.14 g of 4-benzyloxy-2-hydroxybenzaldehyde, 0.125 g of 1,4-diazabicyclo[2,2,2]octane and 0.65 g of acrylonitrile was stirred and heated at 80°-85° C., under argon, for 2 hours. After removal of the solvent, the residual product was dissolved in tetrahydrofuran-ether(1:1), washed with 1N-sodium hydroxide, water, dried, and the solvents evaporated in vacuo. The crude material (1.10 g) was purified by column chromatography on silica gel to afford 0.6 g (45.7%) of 7-(phenylmethoxy)-2H-1-benzopyran-3-carbonitrile, as a colorless solid mp 95°-98° C. (from ethyl acetatehexane).

1. temperatureheated at 80°-85° C., under argon, for 2 hours
2. customAfter removal of the solvent
3. dissolutionthe residual product was dissolved in tetrahydrofuran-ether(1:1)
4. washwashed with 1N-sodium hydroxide, water
5. customdried
6. customthe solvents evaporated in vacuo
7. customThe crude material (1.10 g) was purified by column chromatography on silica gel