反应详情

温度

127 °C

4-Chloro-3', 4'-dimethoxybenzophenone (276.7 g; 1 mol), N-acetyl morpholine (387.6 g; 3 mol) and powdered sodium hydroxide (40.0 g; 1 mol) in n-octane (600 ml) were refluxed under stirring for 10 hours at a column internal temperature of 127° C. The refluxing condensate (3 l/h) was passed through a column packed with molecular sieves (4 A, 150 g). Subsequently, n-octane (450 ml) was distilled off and toluene (1 l) was added. The mixture was heated to 80° C. and extracted once with 500 ml water and twice with 250 ml water. The organic layer was separated, and dried by azeotropic distillation of a part of the solvent (125 ml) under reduced pressure. On cooling to room temperature, crystallisation already started. Under continuous stirring, 750 ml petroleum ether (bp. 58°-63° C.) was added over a period of 30 minutes. After standing overnight, the crystals were collected by vacuum filtration washed with toluene/petroleum ether (1:3; 400 ml) and dried. Yield: 268 g (69.1%). Mp.: 140°-152° C. The product was 98.1% pure and contained 0.9% of the original ketone. The mother liquor contained an additional 25.2 g of the title compound and 42.2 g of the original ketone. The water washings contained 207 g =1.6 mol N-acetyl morpholine.

1. distillationSubsequently, n-octane (450 ml) was distilled off
2. additiontoluene (1 l) was added
3. temperatureThe mixture was heated to 80° C.
4. extractionextracted once with 500 ml water and twice with 250 ml water
5. customThe organic layer was separated
6. dry with materialdried by azeotropic distillation of a part of the solvent (125 ml) under reduced pressure
7. temperatureOn cooling to room temperature
8. customcrystallisation
9. additionUnder continuous stirring, 750 ml petroleum ether (bp. 58°-63° C.) was added over a period of 30 minutes
10. waitAfter standing overnight
11. filtrationthe crystals were collected by vacuum filtration
12. washwashed with toluene/petroleum ether (1:3; 400 ml)
13. customdried