反应详情

A mixture of sulfuric acid (500 ml) and water (100 ml) is heated to 95° and 3-chloro-5-fluorobenzonitrile (94.8 gms) added. After 4 hours the mixture is cooled and poured over ice and water added to make 3.6 L. In 1.2 L portions the mixture is filtered, the solid rinsed with hexane and the aqueous rinsed with hexane (4×120 ml) then extracted with ethyl acetate (2×100 ml). The solid and the ethyl acetate extracts were combined, dried over magnesium sulfate and stripped to give 3-chloro-5-fluorobenzamide as a white solid.

1. temperatureis heated to 95°
2. temperatureAfter 4 hours the mixture is cooled
3. additionadded
4. filtrationIn 1.2 L portions the mixture is filtered
5. washthe solid rinsed with hexane
6. washthe aqueous rinsed with hexane (4×120 ml)
7. extractionthen extracted with ethyl acetate (2×100 ml)
8. dry with materialdried over magnesium sulfate