1,4-Dichlorobutane → Diethyl tetrahydropyridazine-1,2-dicarboxylate

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%.

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)

ORDレコード

ord-e47413391b18435c9654eed6bdfe4a36

出典データセット

uspto-grants-1998_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05739329