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

HRID 226925

반응식

HRID 226925 반응식
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]

참가 물질

4

반응물 2

HCID 8058HexaneHCID 178500756HCID 178500756, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 7416Nitrobenzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8210f470565e403ca28d530672deff0a
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07557213B2

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