Diethyl Ether → 2',4'-Difluoro-2-(2-methoxyethyl)thioacetophenone

HRID 613393

반응식

HRID 613393 반응식
Cl[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][C:6]=1[F:12])=O.COCC[SH:17].C(=O)([O-])[O-].[K+].[K+].[CH3:24][CH2:25][O:26][CH2:27]C>CO>[F:12][C:6]1[CH:7]=[C:8]([F:11])[CH:9]=[CH:10][C:5]=1[C:3](=[S:17])[CH2:2][CH2:24][CH2:25][O:26][CH3:27]

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 11430Potassium CarbonateHCID 5880832-Chloro-1-(2,4-difluorophenyl)ethanoneHCID 30146442-Methoxyethanethiol

생성물 1

HCID 187866342',4'-Difluoro-2-(2-methoxyethyl)thioacetophenone수율 67%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 2-chloro-2',4'-difluoroacetophenone (2.7 g, 0.014 mol) and 2-methoxyethanethiol (J. Med. Chem., 39, 1253(1996)) (1.4 g, 0.015 mol) in methanol (50 ml), potassium carbonate (2.3 g, 0.016 mol) was added under ice cooling, followed by stirring at room temperature for 30 minutes. After the completion of the reaction, the insoluble matter was filtered off and the filtrate was distilled off under reduced pressure. The residue so obtained was diluted with ether, washed with water, dried over magnesium sulfate and distilled off under reduced pressure, whereby 2',4'-difluoro-2-(2-methoxyethyl)thioacetophenone (2.3 g, yield: 67.0%) was obtained as a colorless oil.

후처리

  1. customAfter the completion of the reaction
  2. filtrationthe insoluble matter was filtered off
  3. distillationthe filtrate was distilled off under reduced pressure
  4. customThe residue so obtained
  5. washwashed with water
  6. dry with materialdried over magnesium sulfate
  7. distillationdistilled off under reduced pressure

출처 및 근거

ORD 기록
ord-35d90c19e4874bca853582f35f470620
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06008239

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