Thionyl Chloride → 3-(Pentafluorosulfanyl)benzoyl chloride

HRID 717237ノート

反応式

HRID 717237 の反応式
[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]

参加物

3

反応物 2

HCID 24386Thionyl ChlorideHCID 27792093-(Pentafluorosulfanyl)benzoic acid

生成物 1

HCID 27792133-(Pentafluorosulfanyl)benzoyl chloride

実験手順

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 h. 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.

後処理

  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

出典と根拠

ORDレコード
ord-188d5ae00e6d461d88b6673fc9c6cc4e
出典データセット
uspto-grants-2015_11
特許番号
US09193713B2

反応ノート

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