反应详情

2-Methyl-3-nitrobenzoyl chloride (9.98 grams; 0.05 mole) was dissolved in 35 mls. of dry benzene and the solution was added to a slurry of aluminum chloride (13.3 grams; 0.10 mole) in 40 mls. of dry benzene over a period of 10 minutes. The resulting reaction mixture was stirred at room temperature for 26 1/2 hours, then heated at reflux for 2 hours and cooled to room temperature. The cooled reaction mixture was poured into 200 mls. of dilute hydrochloric acid, stirred for about 15 minutes and allowed to settle. The organic phase was separated and the aqueous phase was back extracted with 200 mls. of benzene. The benzene layer was separated and combined with the organic phase and the combined solution was washed successively with water, a dilute aqueous solution of sodium carbonate, and water. The organic phase was dried over anhydrous sodium sulfate, filtered, concentrated and distilled to obtain 2-methyl-3-nitrobenzophenone (11.45 grams; 95% yield; b.p. 183° C at 2 mm; m.p. 42° C after recrystallization from petroleum ether).

1. customThe resulting reaction mixture
2. temperatureheated
3. temperatureat reflux for 2 hours
4. temperaturecooled to room temperature
5. customThe cooled reaction mixture
6. additionwas poured into 200 mls
7. customThe organic phase was separated
8. extractionthe aqueous phase was back extracted with 200 mls
9. customThe benzene layer was separated
10. washthe combined solution was washed successively with water
11. dry with materialThe organic phase was dried over anhydrous sodium sulfate
12. filtrationfiltered
13. concentrationconcentrated
14. distillationdistilled