Water → 1-(Methylthio)-2-(trifluoromethoxy)benzene

HRID 412447ノート

反応式

HRID 412447 の反応式
CI.[C:3](=O)([O-])[O-].[K+].[K+].[F:9][C:10]([F:20])([F:19])[O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[SH:18].O>CN(C=O)C>[CH3:3][S:18][C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=1[O:11][C:10]([F:9])([F:19])[F:20]

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 27607322-(Trifluoromethoxy)thiophenol

生成物 1

HCID 27815671-(Methylthio)-2-(trifluoromethoxy)benzene収率 90.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of methyl iodide (59.0 g, 0.41 mol) in DMF (150 mL) was added potassium carbonate (23.0 g, 0.16 mol). 2-(Trifluoromethoxy)thiophenol (16.0 g, 0.08 mol) was added in portions during 30 min. The reaction mixture was then stirred vigorously overnight. Water (250 mL) was added. The reaction mixture was extracted with ethyl acetate (2×150 mL). The combined organic phases were washed with a 50% saturated aqueous solution of sodium chloride (4×100 mL), dried (magnesium sulphate), and concentrated in vacuo to give 15.0 g of 1-methylsulfanyl-2-trifluoromethoxybenzene.

後処理

  1. extractionThe reaction mixture was extracted with ethyl acetate (2×150 mL)
  2. washThe combined organic phases were washed with a 50% saturated aqueous solution of sodium chloride (4×100 mL)
  3. dry with materialdried (magnesium sulphate)
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-7c2d53f115284b089a8846ed368d83cd
出典データセット
uspto-grants-2003_05
特許番号
US06562807B2

反応ノート

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