Water → 1,2-Diphenylethane-1,2-dione (2-methylphenyl)-hydrazone

HRID 643288

反応式

HRID 643288 の反応式
Cl.[CH3:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][NH2:10].[C:11]1([C:17](=O)[C:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:19])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.O>C(O)(=O)C>[CH3:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][N:10]=[C:17]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C:18]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=[O:19]

参加物

5

反応物 3

HCID 962WaterHCID 8651BenzilHCID 71554o-Tolylhydrazinium(1+) chloride

生成物 1

HCID 866089501,2-Diphenylethane-1,2-dione (2-methylphenyl)-hydrazone収率 101.8%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 2-methylphenyl hydrazine hydrochloride (0.79 g, 5.0 mmol) and 1,2-diphenyl-ethane-1,2-dione (1.05 g, 5 mmol) in 20 mL of glacial acetic acid was refluxed for 30 min. The reaction was poured into water and extracted with ethyl acetate. The combined organics was dried over MgSO4 and concentrated to give 1.6 gram of 1,2-diphenylethane-1,2-dione (2-methylphenyl)-hydrazone as an orange solid. MS (ESI) m/z 315 ([M+H]+);

後処理

  1. temperaturewas refluxed for 30 min
  2. extractionextracted with ethyl acetate
  3. dry with materialThe combined organics was dried over MgSO4
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-6a58b27c657646648bfad80242fd5e7e
出典データセット
uspto-grants-2010_04
特許番号
US07700595B2

関連ノート

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