2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → HCID 178461867、化合物

HRID 394477ノート

反応式

HRID 394477 の反応式
[C:1]1([CH:7]([NH:9][C:10]2[N:15]=[C:14]([C@H:16]3[C:21]([C:22]4[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:31])([F:30])[F:29])[CH:23]=4)=[N:20][NH:19][C:18](=[O:32])[CH2:17]3)[CH:13]=[CH:12][N:11]=2)[CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl>C(#N)C>[C:1]1([C@@H:7]([NH:9][C:10]2[N:15]=[C:14]([C:16]3[CH:17]=[C:18]([OH:32])[N:19]=[N:20][C:21]=3[C:22]3[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:29])([F:31])[F:30])[CH:23]=3)[CH:13]=[CH:12][N:11]=2)[CH3:8])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 67752,3-Dichloro-5,6-dicyano-1,4-benzoquinoneHCID 70023896(s)-5-[2-(1-Phenylethylamino)pyrimidin-4-yl]-6-(3-trifluoromethylphenyl)-4,5-dihydro-2H-pyridazin-3-one

生成物 1

HCID 178461867HCID 178461867、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Compound 8 (4.24 g, 9.66 mmol), 2,3-dichloro-5,6-dicyano-4-benzoquinone (4.38 g, 19.3 mmol), and acetonitrile (100 mL) were combined and stirred at room temperature under argon for 24 h. The solvent was removed in vacuo and 5% ammonium hydroxide was added. The solution was extracted exhaustively with methylene chloride. The combined organic extracts were dried over anhydrous sodium sulfate and the solvent was removed in vacuo to give a solid. Trituration with hexane-ether gave Compound 9 as a solid: 3.5 g (8.0 mmol, 82%)

後処理

  1. customThe solvent was removed in vacuo and 5% ammonium hydroxide
  2. additionwas added
  3. extractionThe solution was extracted exhaustively with methylene chloride
  4. dry with materialThe combined organic extracts were dried over anhydrous sodium sulfate
  5. customthe solvent was removed in vacuo
  6. customto give a solid

出典と根拠

ORDレコード
ord-283d8006fbdf45f99a66a22d31ef67df
出典データセット
uspto-grants-2003_08
特許番号
US06602872B1

反応ノート

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