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

HRID 2197806
ノート
印刷プレビュー

反応式

HRID 2197806 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-3c511ffeef5342cb9c87511d9885690f
出典データセット
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08338605B2

反応ノート

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