p-Chlorothiophenol → 2-Nitro-4'-chloro diphenyl sulfide

HRID 2185930ノート

反応式

HRID 2185930 の反応式
F[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([SH:18])=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([S:18][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=2[N+:8]([O-:10])=[O:9])=[CH:14][CH:13]=1

参加物

5

反応物 3

HCID 7815p-ChlorothiophenolHCID 11430Potassium CarbonateHCID 738951-Fluoro-2-nitrobenzene

生成物 1

HCID 3653942-Nitro-4'-chloro diphenyl sulfide収率 76.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

2-Fluoronitrobenzene (1.5 g) and 4-chlorothio phenol (1.5 g) were dissolved in ethanol (30 ml) and potassium carbonate (1.4 g) was added thereto, followed by stirring at 60° C. for five hours. Subsequently, the solvent was removed under reduced pressure and the residue was dissolved in water (50 ml). The resultant solution was subjected to extraction with ethyl acetate (30 ml×2). The organic layer was washed sequentially with water and saturated brine and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure. The residue was re-crystallized from diethyl ether, to thereby produce the target compound (2.1 g) as pale-brown crystals.

後処理

  1. customSubsequently, the solvent was removed under reduced pressure
  2. dissolutionthe residue was dissolved in water (50 ml)
  3. extractionThe resultant solution was subjected to extraction with ethyl acetate (30 ml×2)
  4. washThe organic layer was washed sequentially with water and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was removed under reduced pressure
  7. customThe residue was re-crystallized from diethyl ether

出典と根拠

ORDレコード
ord-27df373a2b08438a9fcba83d897ff799
出典データセット
uspto-grants-2002_06
特許番号
US06403607B1

反応ノート

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