反应详情

温度

80 °C

To a slurry of 212.0 g of 2,4-dinitrobenzoic acid in 900 ml of toluene were added with stirring 101.0 g of triethylamine, followed by 159.6 g of bis(2- methoxyethyl)amine. Next 75.7 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 poured slowly into 1000 ml of aqueous 5% NaHCO3 solution with stirring. The precipitate was filtered, washed with water and recrystallized from hot methanol to yield 250.7 g of N,N-bis(2-methoxyethyl)-2,4-dinitrobenzamide, mp 89° C. An additional 19.0 g of material was recovered from the toluene filtrate.

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. customrecrystallized from hot methanol