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Pyridine → 2,5-Bis[(trifluoromethyl)sulfanyl]-1H-pyrrole

HRID 1735642
ノート
印刷プレビュー

反応式

HRID 1735642 の反応式
[F:1][C:2]([F:6])([F:5])[S:3]Cl.[NH:7]1[CH:11]=[CH:10][CH:9]=[CH:8]1.[N:12]1[CH:17]=[CH:16][CH:15]=[CH:14]C=1>C(=O)=O.C(Cl)(Cl)Cl.[Fe]>[F:1][C:2]([F:6])([F:5])[S:3][C:8]1[NH:7][C:11]([S:3][C:2]([F:6])([F:5])[F:1])=[CH:10][CH:9]=1.[F:1][C:2]([F:6])([F:5])[S:3][C:17]1[NH:12][CH:14]=[C:15]([S:3][C:2]([F:6])([F:5])[F:1])[CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

HCID 1049PyridineHCID 8027PyrroleHCID 67900Methanesulfenyl chloride, trifluoro-

生成物 2

HCID 125083162,5-Bis[(trifluoromethyl)sulfanyl]-1H-pyrroleHCID 125083222,4-Bis[(trifluoromethyl)sulfanyl]-1H-pyrrole

試薬・触媒・溶媒 3

HCID 23925Iron触媒
HCID 280
Carbon Dioxide
溶媒
HCID 6212Chloroform溶媒

実験手順

25 g of trifluoromethanesulfenyl chloride was condensed in a pressured bottle in dry ice and 2.34 g of pyrrole in 40 ml of anhydrous chloroform, 12.1 g of pyridine and 0.8 g of iron powder were added. The mixture was then stirred at room temperature for 3 days. It was then filtered to remove insoluble materials. The mixture was washed with water, diluted hydrochloric acid and water again. After evaporation of the solvent, the residue was distilled under vacuum, giving 4.2 g of 2,5-bis(trifluoromethylthio)pyrrole and 3.5 g 2,4-bis(trifluoromethylthio)pyrrole. The total yield was 82%.

後処理

  1. filtrationIt was then filtered
  2. customto remove insoluble materials
  3. washThe mixture was washed with water, diluted hydrochloric acid and water again
  4. customAfter evaporation of the solvent
  5. distillationthe residue was distilled under vacuum

出典と根拠

ORDレコード
ord-97155b9936e34cadbc7e11a8c90454f4
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05538812

反応ノート

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