反应详情

温度

2.5 °C

β-phenylethylamine (0.68 kg) was taken in dry toluene (4.42 L) and sodium bicarbonate (0.612 kg) was added at 30° C. and cooled to 0-5° C. Chloroacetyl chloride was slowly added under nitrogen blanket at 0-10° C., stirred and maintained for 2 hr. After completion of the reaction, water was added slowly and reaction mass was allowed to attain 33±2° C. and the layers were separated. To the aqueous layer toluene was added, stirred and two layers were separated. To the organic layer dil HCl solution (0.653 L DM water+0.272 L con HCl) was added, stirred and two layers were separated. To the organic layer again sodium bicarbonate solution (0.653 L DM water+0.068 kg sodium bicarbonate) was added, stirred and two layers were separated. Water was added to the organic layer, stirred and two layers were separated. From the organic layer toluene was distilled out, methanol was added, heated to 58° C., stirred. To the reaction mass water was added, temperature was maintained at 58° C., stirred for 1-1.5 hr, cool to 30±2° C. for 3 hrs under stirring. Stirring was continued for 3 hrs at 0-5° C. The reaction mass was filtered, washed with water and dried.

1. temperaturemaintained for 2 hr
2. additionwas added slowly
3. customreaction mass
4. customto attain 33±2° C.
5. customthe layers were separated
6. additionTo the aqueous layer toluene was added
7. stirringstirred
8. customtwo layers were separated
9. additionTo the organic layer dil HCl solution (0.653 L DM water+0.272 L con HCl) was added
10. stirringstirred
11. customtwo layers were separated
12. additionTo the organic layer again sodium bicarbonate solution (0.653 L DM water+0.068 kg sodium bicarbonate) was added
13. stirringstirred
14. customtwo layers were separated
15. additionWater was added to the organic layer
16. stirringstirred
17. customtwo layers were separated
18. distillationFrom the organic layer toluene was distilled out
19. additionmethanol was added
20. temperatureheated to 58° C.
21. stirringstirred
22. additionTo the reaction mass water was added
23. temperaturetemperature was maintained at 58° C.
24. stirringstirred for 1-1.5 hr
25. temperaturecool to 30±2° C. for 3 hrs
26. stirringunder stirring
27. stirringStirring
28. filtrationThe reaction mass was filtered
29. washwashed with water
30. customdried