2,5-Hexanedione → 3-(2,5-Dimethylpyrrol-1-yl)-1-phenyl-1H-pyrazole

HRID 83488

反応式

HRID 83488 の反応式
[C:1]1([N:7]2[CH:11]=[CH:10][C:9]([NH2:12])=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:13][C:14](=O)[CH2:15][CH2:16][C:17](=O)[CH3:18]>C(O)(=O)C>[CH3:18][C:17]1[N:12]([C:9]2[CH:10]=[CH:11][N:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[N:8]=2)[C:14]([CH3:13])=[CH:15][CH:16]=1

参加物

4

反応物 2

HCID 80352,5-HexanedioneHCID 5943201-phenyl-1H-pyrazol-3-amine

生成物 1

HCID 712878563-(2,5-Dimethylpyrrol-1-yl)-1-phenyl-1H-pyrazole

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of 1-phenyl-1H-pyrazol-3-ylamine (32.7 g) in acetic acid (330 ml) was added 2,5-hexanedione (25 ml), and the mixture was stirred for 3 hours at reflux. This reaction solution was cooled to room temperature, and then acetic acid was concentrated under reduced pressure, and then toluene (100 ml) was added thereto, and the mixture was further concentrated. The resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate 100/1 to 20/1) to give the titled compound (41.8 g).

後処理

  1. temperatureat reflux
  2. concentrationacetic acid was concentrated under reduced pressure
  3. additiontoluene (100 ml) was added
  4. concentrationthe mixture was further concentrated
  5. customThe resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate 100/1 to 20/1)

出典と根拠

ORDレコード
ord-d6cc9c75209b44ca98adb1e56a69c812
出典データセット
uspto-grants-2014_09
特許番号
US08846746B2

関連ノート

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