HRID1598948

反应详情

EQUATION

反应方程式

HRID 1598948 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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%.

WORKUP

后处理

  1. customInto a 500-ml, four-necked flask equipped with a reflux condenser, a stirrer
  2. temperaturegradually warmed up to 50°-60° C. and aged for 3 hours
  3. customAfter completion of the reaction
  4. temperaturethe reaction mixture was cooled
  5. filtrationfiltered
  6. customto remove the solid matters
  7. customafter which the solvent was removed by distillation under reduced pressure
  8. customThe residue obtained
  9. distillationwas distilled under reduced pressure (110° C./1 mmHg)