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

HRID 643288

반응식

HRID 643288 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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]+);

후처리

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

출처 및 근거

ORD 기록
ord-6a58b27c657646648bfad80242fd5e7e
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07700595B2

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