反应详情

温度

80 °C

To a slurry of 215.1 g of 2,4-dinitrobenzoic acid in 1000 ml of toluene was added with stirring 196.2 g of morpholine. Next 76.5 g of phosphorus oxychloride was added dropwise at such a rate to maintain the reaction temperature below 90° C. The mixture was refluxed for 5 hrs, cooled to 80° C., and slowly poured into 1000 ml of aqueous 5% NaHCO3 solution with stirring. The precipitate was filtered, washed with water and dried to yield 231.7 g of N-(2,4-dinitrobenzoyl)morpholine, mp 159°-161° C.

1. temperatureto maintain the reaction temperature below 90° C
2. temperatureThe mixture was refluxed for 5 hrs
3. filtrationThe precipitate was filtered
4. washwashed with water
5. customdried