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

HRID 1633937

반응식

HRID 1633937 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

HCID 27815671-(Methylthio)-2-(trifluoromethoxy)benzene수율 90.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a02848819e29437796a1a6450e27b0e5
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06503949B1

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