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Sodium Carbonate → 1-(2-Fluoro-phenylsulfanyl)-4-methyl-2-nitro-benzene

HRID 2358641
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HRID 2358641 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5](OS(C(F)(F)F)(=O)=O)=[C:4]([N+:16]([O-:18])=[O:17])[CH:3]=1.[F:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[SH:26].C([O-])([O-])=O.[Na+].[Na+]>CCO>[F:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[S:26][C:5]1[CH:6]=[CH:7][C:2]([CH3:1])=[CH:3][C:4]=1[N+:16]([O-:18])=[O:17]
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참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 5202162-FluorothiophenolHCID 713468894-Methyl-2-nitrophenyl trifluoromethanesulfonate

생성물 1

HCID 684579081-(2-Fluoro-phenylsulfanyl)-4-methyl-2-nitro-benzene

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

The product from Example 4a (1.50 g, 5.3 mmol) and 2-fluorobenzenethiol (0.56 mL, 5.3 mmol) in EtOH (15 mL) was added aqueous Na2CO3 solution (0.563 g, 5.3 mmol) dropwise at room temperature. The mixture was heated to reflux fluxed for 1 hour, and then evaporated. The residue was diluted with EtOAc, washed with H2O, 5% KOH and brine, dried over MgSO4, filtered and concentrated under vacuum giving the title compound as yellow crystal, which was purified by washing with cold n-hexane to give the title product as yellow crystal (1.15 g, 83%).

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux
  3. customevaporated
  4. additionThe residue was diluted with EtOAc
  5. washwashed with H2O, 5% KOH and brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-ca63dc1600c84b7f909db5487a12adb0
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07763731B2

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