反应详情

温度

0 °C

To 123 kg of ethanol, 25.0 kg (167 mol) of sodium iodide and 14.2 kg (152 mol) of α-chloroacetamide were added and the resultant mixture was heated to 77° C. and was stirred for 3 hours. To the resultant suspension, 58.2 kg (130 mol) of 69% toluene solution of diethyl 2-benzyloxycarbonylaminomalonate was added, followed by cooling the resultant mixture to 0° C. Thereto, 89.1 kg (262 mol) of 20% ethanol solution of sodium ethoxide was dropped for 3 hours while maintaining the temperature at 0° C. After the reaction mixture was stirred for 3 hours at 0° C., the reaction was quenched by adding 7.9 kg of acetic acid and 15.1 kg of 85% phosphoric acid to the reaction mixture and the solvent was distilled off under reduced pressure. To the reaction mixture, 200 kg of toluene and 80 kg of water were added and the phase separation of the reaction mixture was performed. After the organic phase was washed with water 3 times, it was quantitatively analyzed and the yield of 2-benzyloxycarbonylamino-2-ethoxycarbonyl succinimide was found to be 87.5%. This solution was concentrated and then was recrystallized with toluene and ethanol to thereby obtaining 30 kg (yield: 72%) of 2-benzyloxycarbonylamino-2-ethoxycarbonyl succinimide as a white crystal.

1. stirringAfter the reaction mixture was stirred for 3 hours at 0° C.
2. customthe reaction was quenched
3. additionby adding 7.9 kg of acetic acid and 15.1 kg of 85% phosphoric acid to the reaction mixture
4. distillationthe solvent was distilled off under reduced pressure
5. additionTo the reaction mixture, 200 kg of toluene and 80 kg of water were added
6. customthe phase separation of the reaction mixture
7. washAfter the organic phase was washed with water 3 times, it
8. concentrationThis solution was concentrated
9. customwas recrystallized with toluene and ethanol