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

HRID 1633937ノート

反応式

HRID 1633937 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 minutes. 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 extracted with a 50% saturated aqueous solution of sodium chloride (4×100 mL), dried (MgSO4), 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. extractionThe combined organic phases were extracted with a 50% saturated aqueous solution of sodium chloride (4×100 mL)
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-a02848819e29437796a1a6450e27b0e5
出典データセット
uspto-grants-2003_01
特許番号
US06503949B1

反応ノート

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