4-Chloro-1,2-diaminobenzene → HCID 136059437、化合物

HRID 499160ノート

反応式

HRID 499160 の反応式
[O:1]=[C:2]1[NH:7][N:6]=[C:5]([C:8](O)=O)[CH:4]=[CH:3]1.[Cl:11][C:12]1[CH:13]=[C:14]([NH2:19])[C:15]([NH2:18])=[CH:16][CH:17]=1.C([O-])(O)=O.[Na+]>O>[Cl:11][C:12]1[CH:17]=[CH:16][C:15]2[N:18]=[C:8]([C:5]3[CH:4]=[CH:3][C:2](=[O:1])[NH:7][N:6]=3)[NH:19][C:14]=2[CH:13]=1

参加物

5

反応物 3

HCID 72634-Chloro-1,2-diaminobenzeneHCID 3059706-Hydroxypyridazine-3-carboxylic AcidHCID 516892Sodium Bicarbonate

生成物 1

HCID 136059437HCID 136059437、化合物収率 17%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 6-oxo-1,6-dihydropyridazine-3-carboxylic acid (0.790 g, 5.000 mmol) and 4-chlorobenzene-1,2-diamine (0.720 g, 5.000 mmol) was added to pre-heated (150° C.) polyphosphoric acid (5 g) with stirring, and the reaction was stirred at 150 C for 2 hours. Water was added to the reaction mixture, and the resulting solution was neutralized with NaHCO3, and extracted with ethyl acetate. The organic phase was dried and evaporated to afford 6-(6-chloro-1H-benzoimidazol-2-yl)-2H-pyridazin-3-one as a dark solid (0.210 g, 0.85 mmol, 17% yield).

後処理

  1. additionwas added
  2. stirringthe reaction was stirred at 150 C for 2 hours
  3. extractionextracted with ethyl acetate
  4. customThe organic phase was dried
  5. customevaporated

出典と根拠

ORDレコード
ord-6a8726e5d64d4efe91041050fa9e998d
出典データセット
uspto-grants-2010_08
特許番号
US07767677B2

反応ノート

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