反应详情

温度

50 °C

In a 2.5 1 sulfonation flask, 900 ml of a solution (1 mol) of 2-dimethylamino-1 -(4-morpholino-phenyl)butan-1 -one according to b) above are heated again to 50° C. 179.7 g (1.05 mol) of benzyl bromide are then added dropwise over 20 minutes. The mixture is stirred for 3 to 4 hours at 50° C. until the thin layer chromatogram shows that there is no educt left. The temperature is raised to 60° C. and then 80 g (2 mol) of sodium hydroxide powder are added in increments over 45 minutes. The mixture is then stirred for another 1 to 2 hours at 50° C. until the thin layer chromatogram shows that there is no educt left. The reaction mixture is charged with 150 ml of water and stirred. The water phase is separated and the organic phase is concentrated on a vacuum rotary evaporator. 378.3 g of the yellowish crude product of 2-benzyl-2-dimethylamino-1 -(4-morpholinophenyl)butan-1 -one having a melting point from 102° C. to 110° C. remain in the flask. The crude product is dissolved hot in 600 ml of ethanol, cooled, crystallised, filtered and then washed with cold ethanol. The crystals are dried. They melt at 114° C. to 115° C., and gas chromatogram as well as thin layer chromatogram show them to be pure. The yield is 299.0 g of 2-benzyl-2-dimethylamino-1-(4-morpholinophenyl)butan-1-one. A further 22.4 g of pure product can be isolated from the mother liquor. The 1H-NMR spectrum of the pure product corresponds to that of the indicated structure.

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2. temperatureThe temperature is raised to 60° C.
3. stirringThe mixture is then stirred for another 1 to 2 hours at 50° C. until the thin layer chromatogram
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5. stirringstirred
6. customThe water phase is separated
7. concentrationthe organic phase is concentrated on a vacuum rotary evaporator
8. customfrom 102° C. to 110° C.
9. dissolutionThe crude product is dissolved hot in 600 ml of ethanol
10. temperaturecooled
11. customcrystallised
12. filtrationfiltered
13. washwashed with cold ethanol
14. customThe crystals are dried
15. custommelt at 114° C. to 115° C.