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

HRID 1598948
ノート
印刷プレビュー

反応式

HRID 1598948 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 281963Diethyl tetrahydropyridazine-1,2-dicarboxylate収率 143.3%

試薬・触媒・溶媒 1

HCID 66611,3-Dimethyl-2-imidazolidinone溶媒

実験手順

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%.

後処理

  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)

出典と根拠

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

反応ノート

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