Methyl iodide → 2-Trifluoromethylthioanisole
反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[SH:9].[C:12](=O)([O-])[O-].[K+].[K+].IC>CN(C=O)C>[CH3:12][S:9][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[C:2]([F:1])([F:10])[F:11]参加物
5
実験手順
Dissolve 2-trifluoromethyl-benzenethiol (10 g, 56 mmol), potassium carbonate (25 g, 180 mmol), iodomethane (11 mL, 177 mmol) in DMF (100 mL). Stir for 12 hours. Filter the suspension through a pad of silica gel and elute with ethyl acetate (500 mL). Evaporate half of the solvent and wash the remaining solution with 10% aqueous LiCl (100 mL). Dry with MgSO4 and evaporate solvent. Chromatograph the residue on a SiO2 column eluting with hexane to give 9.5 g of 1-methylsulfanyl-2-trifluoromethyl-benzene (88%).
後処理
- filtrationFilter the suspension through a pad of silica gel
- washelute with ethyl acetate (500 mL)
- customEvaporate half of the solvent
- washwash the remaining solution with 10% aqueous LiCl (100 mL)
- dry with materialDry with MgSO4
- customevaporate solvent
- washChromatograph the residue on a SiO2 column eluting with hexane
出典と根拠
- ORDレコード
- ord-1dcc37024a1b4713881d06f1f0f0ff72
- 出典データセット
- uspto-grants-2009_09
- 特許番号
- US07585977B2
反応ノート
読み込み中…