반응 #1686130

반응 방정식

diethyl hydrazinedicarboxylate

1,4-dichlorobutane

potassium hydroxide

→

diethyl hexahydropyridazine-1,2-dicarboxylate

수율 143.3%

용매

1,3-dimethylimidazolidinone

반응 조건

후처리

1. 1
   기타Into a 500-ml, four-necked flask equipped with a reflux condenser, a stirrer
2. 2
   온도gradually warmed up to 50°-60° C. and aged for 3 hours
3. 3
   기타After completion of the reaction
4. 4
   온도the reaction mixture was cooled
5. 5
   여과filtered
6. 6
   기타to remove the solid matters
7. 7
   기타after which the solvent was removed by distillation under reduced pressure
8. 8
   기타The residue obtained
9. 9
   workup.DISTILLATIONwas distilled under reduced pressure (110° C./1 mmHg)

실험 절차

Into a 500-ml, four-necked flask equipped with a reflux condenser, a stirrer and a thermometer were charged 35.2 g (0.2 mole) of diethyl hydrazinedicarboxylate, 25.9 g (0.204 mole) of 1,4-dichlorobutane, 200 ml of 1,3-dimethylimidazolidinone and 22.4 g (0.4 mole) of potassium hydroxide, gradually warmed up to 50°-60° C. and aged for 3 hours. After completion of the reaction, the reaction mixture was cooled and filtered to remove the solid matters, after which the solvent was removed by distillation under reduced pressure. The residue obtained was distilled under reduced pressure (110° C./1 mmHg) to obtain 33.0 g of diethyl hexahydropyridazine-1,2-dicarboxylate. The yield was 72%.

출처