Hexane → 3-(3,4-dimethyl-benzoyl)-6-trifluoromethyl-1H-quinolin-4-one

HRID 226925

反応式

HRID 226925 の反応式
CO[C:3](=[O:27])[C:4]([C:17](=[O:26])[C:18]1[CH:23]=[CH:22][C:21]([CH3:24])=[C:20]([CH3:25])[CH:19]=1)=[CH:5][NH:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]([F:16])([F:15])[F:14])=[CH:9][CH:8]=1.CCCCCC>[N+](C1C=CC=CC=1)([O-])=O>[CH3:25][C:20]1[CH:19]=[C:18]([CH:23]=[CH:22][C:21]=1[CH3:24])[C:17]([C:4]1[C:3](=[O:27])[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([C:13]([F:16])([F:14])[F:15])[CH:11]=2)[NH:6][CH:5]=1)=[O:26]

参加物

4

反応物 2

HCID 8058HexaneHCID 178500756HCID 178500756、化合物

生成物 1

HCID 577545723-(3,4-dimethyl-benzoyl)-6-trifluoromethyl-1H-quinolin-4-one収率 83.3%

試薬・触媒・溶媒 1

HCID 7416Nitrobenzene溶媒

実験手順

2-(3,4-dimethyl-benzoyl)-3-(4-trifluoromethyl-phenylamino)-acrylic acid methyl ester 2c (151 mg, 0.40 mmol) was refluxed in 5 mL of nitrobenzene for 3 h, then cooled down and to it was added 10 mL of hexane. The crude product precipitated out of solution and was isolated by filtration. The crude product was washed with hexane to give 115 mg of 3-(3,4-dimethyl-benzoyl)-6-trifluoromethyl-1H-quinolin-4-one as off-white crystals 3b: LC-MSD, m/z for C19H14F3NO2, [M+H]+=346.4,; HPLC retention time: 2.3 min.

後処理

  1. temperaturecooled down and to it
  2. customThe crude product precipitated out of solution
  3. customwas isolated by filtration
  4. washThe crude product was washed with hexane

出典と根拠

ORDレコード
ord-8210f470565e403ca28d530672deff0a
出典データセット
uspto-grants-2009_07
特許番号
US07557213B2

関連ノート

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