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Trifluoroacetamide → N-(4-Bromobenzenesulfinyl)-2,2,2-trifluoroacetamide

HRID 1485629
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HRID 1485629 반응식
C([Li])CCC.[F:6][C:7]([F:12])([F:11])[C:8]([NH2:10])=[O:9].[Br:13][C:14]1[CH:19]=[CH:18][C:17]([S:20](Cl)=[O:21])=[CH:16][CH:15]=1>O1CCCC1>[Br:13][C:14]1[CH:19]=[CH:18][C:17]([S:20]([NH:10][C:8](=[O:9])[C:7]([F:12])([F:11])[F:6])=[O:21])=[CH:16][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 67717TrifluoroacetamideHCID 109775414-Bromobenzenesulfinic chlorideHCID 178418339Butyllithium

생성물 1

HCID 118863945N-(4-Bromobenzenesulfinyl)-2,2,2-trifluoroacetamide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Thionyl chloride (0.53 mL) is added to an ice-cooled solution of 4-bromobenzenesulfinic acid (400 mg) in dichloromethane (15 mL) under an argon atmosphere. The reaction mixture is stirred for 2 h at 0° C., warmed to room temperature, and stirred for an additional 30 min. The mixture is concentrated and the residue is co-evaporated twice with toluene to give crude 4-bromobenzenesulfinic chloride, which is dissolved in tetrahydrofuran (3 mL) and cooled to −78° C. n-Butyllithium (1.6 M in hexane; 2.26 mL) is added to 2,2,2-trifluoroacetamide (205 mg) in tetrahydrofuran (3 mL) at −78° C. and the reaction mixture is stirred for 10 min. The mixture is added to the 4-bromobenzenesulfinic chloride solution at −78° C. and the reaction mixture is stirred for 1 h. The cooling bath is removed and the reaction is quenched by addition of water and brine. The aqueous layer is extracted with ethyl acetate and the combined extracts are washed with brine and concentrated in vacuo to give the title compound which is used for the next step without further purification. LC (method 1): tR=0.92 min; Mass spectrum (ESI+): m/z=314 [M−H]−.

후처리

  1. stirringthe reaction mixture is stirred for 1 h
  2. customThe cooling bath is removed
  3. customthe reaction is quenched by addition of water and brine
  4. extractionThe aqueous layer is extracted with ethyl acetate
  5. washthe combined extracts are washed with brine
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-71ecedd187a243679ed991c3ef07ecef
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09422312B2

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