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Dimethylformamide → 4'-Chlorobiphenyl-4-sulfonyl chloride

HRID 413360
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HRID 413360 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([S:14]([OH:17])(=O)=[O:15])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.CN(C)C=O.S(Cl)([Cl:25])=O>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([S:14]([Cl:25])(=[O:17])=[O:15])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 154291414'-Chloro[1,1'-biphenyl]-4-sulfonic acid

생성물 1

HCID 27947454'-Chlorobiphenyl-4-sulfonyl chloride

실험 절차

To a solution of 4′-chlorobiphenyl-4-sulfonic acid 12a (15.1 g ,78.1 mmol)in thionyl chloride (150 mL) is added a catalytic amount of N,N-dimethylformamide (0.3 mL). The reaction mixture is heated to reflux for 4 hr. The mixture is then cooled to room temperature, and concentrated under reduced pressure. Toluene is then added and the mixture is concentrated under reduced pressure. The solid crude product is then recrystallized with ethyl acetate and hexanes to give the solid desired product.

후처리

  1. temperatureThe reaction mixture is heated
이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
  • temperatureto reflux for 4 hr
  • concentrationconcentrated under reduced pressure
  • additionToluene is then added
  • concentrationthe mixture is concentrated under reduced pressure
  • customThe solid crude product is then recrystallized with ethyl acetate and hexanes
  • 출처 및 근거

    ORD 기록
    ord-ecfe949a310d4785bc775841b1b5dfff
    출처 데이터셋
    uspto-grants-2003_05
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06566381B1

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