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

HRID 1598948

반응식

HRID 1598948 반응식
[N:1]([C:8](OCC)=O)([C:3]([O:5][CH2:6][CH3:7])=[O:4])[NH2:2].Cl[CH2:14][CH2:15][CH2:16]CCl.[OH-:19].[K+]>CN1CCN(C)C1=O>[N:1]1([C:3]([O:5][CH2:6][CH3:7])=[O:4])[CH2:8][CH2:14][CH2:15][CH2:16][N:2]1[C:3]([O:5][CH2:6][CH3:7])=[O:19]

참가 물질

5

반응물 3

HCID 80591,4-DichlorobutaneHCID 14797Potassium HydroxideHCID 12066737Diethyl hydrazinedicarboxylate

생성물 1

HCID 281963Diethyl tetrahydropyridazine-1,2-dicarboxylate수율 143.3%

시약·촉매·용매 1

HCID 66611,3-Dimethyl-2-imidazolidinone용매

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%.

후처리

  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)

출처 및 근거

ORD 기록
ord-e47413391b18435c9654eed6bdfe4a36
출처 데이터셋
uspto-grants-1998_04
특허 번호
US05739329

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