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

HRID 967649노트

반응식

HRID 967649 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 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.

후처리

  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

출처 및 근거

ORD 기록
ord-281f2df20ac44ab09d07fd512ca403a4
출처 데이터셋
uspto-grants-2005_10
특허 번호
US06953812B2

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