2-Fluoro-5-nitrobenzotrifluoride → 1-(Methylsulphonyl)-4-nitro-2-(trifluoromethyl)benzene

HRID 396799

反応式

HRID 396799 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[C:11]([F:14])([F:13])[F:12].[CH3:15][S:16]([O-:18])=[O:17].[Na+]>CS(C)=O>[CH3:15][S:16]([C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[C:11]([F:14])([F:13])[F:12])(=[O:18])=[O:17]

参加物

4

反応物 2

HCID 949542-Fluoro-5-nitrobenzotrifluorideHCID 2733271Sodium methanesulfinate

生成物 1

HCID 206051531-(Methylsulphonyl)-4-nitro-2-(trifluoromethyl)benzene収率 57.9%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
130 °C

実験手順

A mixture of 2-fluoro-5-nitrobenzotrifluoride (2.09 g, 10 mmol) and sodium methanesulfinate (1.32 g, 11 mmol) in DMSO (20 mL) was heated at 130° C. for 17.5 hours. After cooling down to room temperature, the mixture was poured into ice-water. The whole was extracted with ethyl acetate (30 mL×2), the combined organic layer washed with water, brine, dried over MgSO4, and concentrated in vacuo. The residue was crystallized from hexane to give the subtitle compound (1.56 g, 57.8%, yield).

後処理

  1. temperatureAfter cooling down to room temperature
  2. extractionThe whole was extracted with ethyl acetate (30 mL×2)
  3. washthe combined organic layer washed with water, brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe residue was crystallized from hexane

出典と根拠

ORDレコード
ord-72ceefca634e4569a06b77505b891b93
出典データセット
uspto-grants-2003_08
特許番号
US06608095B2

関連ノート

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