反应详情

To a solution of 3-ethoxy-4-methoxybenzamide (3.30 g) in pyridine (33 mL) was added phosphorus oxychloride (1.73 mL) under ice-water cooling, and the mixture was stirred for 2 hours at ambient temperature. After evaporation of the solvent, the residue was partitioned between ethyl acetate and water under ice-water cooling. The separated organic layer was washed with 1N-hydrochloric acid, water and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by a silica gel column chromatography eluting with a mixture of hexane and ethyl acetate (5:1 to 4:1) to give 3-ethoxy-4-methoxybenzonitrile as colorless powders (2.83 g).

1. customAfter evaporation of the solvent
2. customthe residue was partitioned between ethyl acetate and water under ice-water cooling
3. washThe separated organic layer was washed with 1N-hydrochloric acid, water and brine
4. dry with materialdried over magnesium sulfate
5. customevaporated in vacuo
6. customThe residue was purified by a silica gel column chromatography
7. washeluting with a mixture of hexane and ethyl acetate (5:1 to 4:1)