反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[S:10]([OH:12])=[O:11].IC.[CH2:15](N(C(C)C)C(C)C)C>CN(C=O)C>[F:9][C:5]1[CH:4]=[C:3]([S:10]([CH3:15])(=[O:12])=[O:11])[C:2]([F:1])=[CH:7][C:6]=1[F:8]参加物
5
実験手順
To a solution of 2,4,5-trifluorobenzenesulfinic acid (34 g, 173 mmol), in DMF (200 mL), was added iodomethane (21.6 mL, 347 mmol), and N-ethyl-N-isopropylpropan-2-amine (60.5 mL, 347 mmol). The reaction mixture was stirred overnight at ambient temperature. The reaction was concentrated and partitioned between water and ethyl acetate and extracted with CH2Cl2. The combined organic layers were concentrated and purified over silica gel (15-100% EtOAc in hexanes) to afford 1,2,4-trifluoro-5-(methylsulfonyl)benzene (25.8 g, 123 mmol, 71% yield) as yellow solid.
後処理
- concentrationThe reaction was concentrated
- custompartitioned between water and ethyl acetate
- extractionextracted with CH2Cl2
- concentrationThe combined organic layers were concentrated
- custompurified over silica gel (15-100% EtOAc in hexanes)
出典と根拠
- ORDレコード
- ord-4d3484d721434e5da22963726d069d9d
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08754226B2
関連ノート
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