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

HRID 1735642
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반응식

HRID 1735642 반응식
[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
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참가 물질

8

반응물 3

HCID 1049PyridineHCID 8027PyrroleHCID 67900Methanesulfenyl chloride, trifluoro-

생성물 2

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

시약·촉매·용매 3

HCID 23925Iron촉매
HCID 280
Carbon Dioxide
용매
HCID 6212Chloroform용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-97155b9936e34cadbc7e11a8c90454f4
출처 데이터셋
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05538812

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