Thionyl Chloride → 3-(Pentafluorosulfanyl)benzoyl chloride

HRID 452960노트

반응식

HRID 452960 반응식
[CH:1]1[CH:6]=[C:5]([S:7]([F:12])([F:11])([F:10])([F:9])[F:8])[CH:4]=[C:3]([C:13]([OH:15])=O)[CH:2]=1.O=S(Cl)[Cl:18]>>[F:8][S:7]([F:12])([F:11])([F:10])([F:9])[C:5]1[CH:4]=[C:3]([CH:2]=[CH:1][CH:6]=1)[C:13]([Cl:18])=[O:15]

참가 물질

3

반응물 2

HCID 24386Thionyl ChlorideHCID 27792093-(Pentafluorosulfanyl)benzoic acid

생성물 1

HCID 27792133-(Pentafluorosulfanyl)benzoyl chloride

실험 절차

A mixture of 3-(pentafluorothio)benzoic acid (Apollo Scientific, 0.42 g, 1.7 mmol) and SOCl2 (1.2 mL, 16.9 mmol) was warmed to reflux and was allowed to stir for 2 hours. The mixture was cooled to ambient temperature and concentrated under reduced pressure. The residue was dissolved in toluene (5 mL) and was concentrated under reduced pressure. This dilution with toluene and concentration was repeated two additional times to remove residual thionyl chloride and afford 3-(pentafluoro-λ6-sulfanyl)benzoyl chloride that was used directly below.

후처리

  1. temperaturewas warmed
  2. temperatureto reflux
  3. concentrationconcentrated under reduced pressure
  4. dissolutionThe residue was dissolved in toluene (5 mL)
  5. concentrationwas concentrated under reduced pressure
  6. concentrationThis dilution with toluene and concentration
  7. customto remove residual thionyl chloride

출처 및 근거

ORD 기록
ord-f7cfb2a7531d48f7bc9721c8eb7f4cd5
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08492371B2

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