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

HRID 613393

反応式

HRID 613393 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-35d90c19e4874bca853582f35f470620
出典データセット
uspto-grants-1999_12
特許番号
US06008239

関連ノート

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