Methyl iodide → 2-Trifluoromethylthioanisole
반응식
[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]참가 물질
5
실험 절차
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 ne). 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%).
후처리
- filtrationFilter the suspension through a pad of silica gel
- washelute with ethyl acetate (500 ne)
- 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
출처 및 근거
- ORD 기록
- ord-8bc369078a324b31b484c7f40d2e3c9f
- 출처 데이터셋
- uspto-grants-2008_07
- 특허 번호
- US07399867B2
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