Iodine → 1,2-Bis(2-(trifluoromethyl)phenyl)disulfane

HRID 335212

反応式

HRID 335212 の反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[SH:9].II>C(#N)C>[F:11][C:2]([F:1])([F:10])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[S:9][S:9][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[C:2]([F:11])([F:10])[F:1]

参加物

4

反応物 2

HCID 807IodineHCID 27778892-(Trifluoromethyl)benzenethiol

生成物 1

HCID 113256811,2-Bis(2-(trifluoromethyl)phenyl)disulfane収率 88.3%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of 2-(trifluoromethyl)benzenethiol (0.185 mL, 1.40 mmol) in wet acetonitrile (1:5 water/acetonitrile) was added Iodine (0.178 g, 0.702 mmol) and allowed to stir over night at room temperature. The reaction was concentrated, then diluted with EtOAc and quenched with aqueous sodium thiosulfate, extracted and dried organic with brine, Na2SO4, filtered and concentrated to afford the title compound (219 mg, 44% yield) as a colorless oil.

後処理

  1. concentrationThe reaction was concentrated
  2. additiondiluted with EtOAc
  3. customquenched with aqueous sodium thiosulfate
  4. extractionextracted and dried organic with brine, Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-8686f30af43d42c38c3c3a12ee695cf5
出典データセット
uspto-grants-2014_11
特許番号
US08883828B2

関連ノート

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