Dimethylformamide → 4'-Bromobiphenyl-4-sulfonyl chloride

HRID 413363노트

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HRID 413363 반응식
[Br: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>>[Br: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 물질

4

반응물 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 45247074-BROMO-4'-SULFOBIPHENYL

생성물 1

HCID 27568454'-Bromobiphenyl-4-sulfonyl chloride

실험 절차

To a solution of 4′-bromobiphenyl-4-sulfonic acid 13a (18.8 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
  2. temperatureto reflux for 4 hr
  3. concentrationconcentrated under reduced pressure
  4. additionToluene is then added
  5. concentrationthe mixture is concentrated under reduced pressure
  6. customThe solid crude product is then recrystallized with ethyl acetate and hexanes

출처 및 근거

ORD 기록
ord-33ab656c678a47d1bde8b4b0f7f06a41
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06566381B1

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