Water → 8-Methyl-3,4-diphenylcinnoline

HRID 643289

반응식

HRID 643289 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][N:9]=[C:10]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:11]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=O.O>S(=O)(=O)(O)O>[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]2[C:3]=1[N:8]=[N:9][C:10]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[C:11]2[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

참가 물질

4

반응물 2

HCID 962WaterHCID 866089501,2-Diphenylethane-1,2-dione (2-methylphenyl)-hydrazone

생성물 1

HCID 118567038-Methyl-3,4-diphenylcinnoline수율 5.3%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

1,2-Diphenylethane-1,2-dione (2-methylphenyl)-hydrazone (0.50 g, 1.59 mmol) was dissolved in 70% of sulfuric acid (10 mL) and the reaction was stirred at room temperature overnight. The reaction was poured into iced water and extracted with ethyl acetate. The combined organics was dried over MgSO4 and concentrated. The material was purified via column chromatography using 5-100% ethyl actetate in hexane as the eluent to yield 0.025 g of the title compound as an orange solid. MS (ESI) m/z 297([M+H]+); HRMS (ESI, [M+H]+) 297.1406.

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialThe combined organics was dried over MgSO4
  3. concentrationconcentrated
  4. customThe material was purified via column chromatography

출처 및 근거

ORD 기록
ord-25bccea003be4a56baf96c772ab9bc1c
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07700595B2

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