2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → HCID 23471598、化合物

HRID 128019ノート

反応式

HRID 128019 の反応式
[CH3:1][CH:2]1[C:7]([C:8]2[CH:9]=[C:10]3[C:15](=[CH:16][CH:17]=2)[N:14]([CH3:18])[C:13](=[O:19])[CH2:12][CH2:11]3)=[N:6][NH:5][C:4](=[O:20])[CH2:3]1.ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl>C1C=CC=CC=1>[CH3:1][CH:2]1[C:7]([C:8]2[CH:9]=[C:10]3[C:15](=[CH:16][CH:17]=2)[N:14]([CH3:18])[C:13](=[O:19])[CH:12]=[CH:11]3)=[N:6][NH:5][C:4](=[O:20])[CH2:3]1

参加物

4

反応物 2

HCID 67752,3-Dichloro-5,6-dicyano-1,4-benzoquinoneHCID 129826Y 590

生成物 1

HCID 23471598HCID 23471598、化合物収率 28%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of 5.4 g of 6-(5-methyl-3-oxo-2,3,4,5-tetrahydropyridazin-6-yl)-1-methyl-1,2,3,4-tetrahydroquinolin-2-one, 5.5 g of 2,3-dichloro-5,6-dicyano-1,4-benzoquinone and 500 ml of benzene was heated under reflux for 48 hours. After cooling, the precipitated crystals were filtered off. The filtrate was washed with a 10% sodium hydroxide solution and dried over sodium sulfate. The solvent was distilled off under reduced pressure. The residue and the crystals were combined and purified by using a column chromatograph. The resulting crystals were recrystallized from methanol to give 1.5 g of 6-(5-methyl-3-oxo-2,3,4,5-tetrahydropyridazin-6-yl)-1-methyl-1,2-dihydroquinolin-2-one, melting at 248°-251° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 48 hours
  3. temperatureAfter cooling
  4. filtrationthe precipitated crystals were filtered off
  5. washThe filtrate was washed with a 10% sodium hydroxide solution
  6. dry with materialdried over sodium sulfate
  7. distillationThe solvent was distilled off under reduced pressure
  8. custompurified
  9. customThe resulting crystals were recrystallized from methanol

出典と根拠

ORDレコード
ord-23aebc49575048f78dc97f67179657f2
出典データセット
uspto-grants-1981_03
特許番号
US04258185

反応ノート

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