反应详情

温度

3 °C

Diethylamine (9.5 L) was charged into a 20 L glass-lined reactor and cooled to 3° C. Chloroacetic acid (1.21 kg) in MTBE (1.8 L) was added over 1 hour with cooling—the temperature rose to 16° C. during the addition. The mixture was warmed to 20° C., stirred over night and concentrated on rotary evaporator giving yellow oil. This oil was re-concentrated with iPrOAc, mixed with iPrOAc (4.5 L) and stirred over night. The off-white hygroscopic precipitate was filtered, washed with iPrOAc (1.5 L) and immediately placed into a drying cabinet to avoid deliquescence. After drying, titled product was obtained (820 g, Y=49%).

1. additionrose to 16° C. during the addition
2. temperatureThe mixture was warmed to 20° C.
3. concentrationconcentrated on rotary evaporator
4. customgiving yellow oil
5. concentrationThis oil was re-concentrated with iPrOAc
6. additionmixed with iPrOAc (4.5 L)
7. stirringstirred over night
8. filtrationThe off-white hygroscopic precipitate was filtered
9. washwashed with iPrOAc (1.5 L)
10. customAfter drying