Methanol → Methyl 4,5-difluoro-2-hydroxybenzoate
반응식
[F:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([OH:12])[CH:3]=1.OS(O)(=O)=O.[CH3:18]O>>[F:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([O:8][CH3:18])=[O:7])=[C:4]([OH:12])[CH:3]=1참가 물질
4
실험 절차
A mixture of 4,5-difluoro-2-hydroxybenzoic acid (20 mmol), methanol (100 ml) and concentrated H2SO4 (5 ml) was refluxed for 48 h. Then, the reaction mixture was concentrated. The residue was dissolved in ethyl acetate, washed with brine and a saturated NaHCO3 solution and neutralized with citric acid. The organic layer was dried over MgSO4 and concentrated in vacuo to give the product. Yield: 2.8 g (97% purity, 74% yield).
후처리
- temperaturewas refluxed for 48 h
- concentrationThen, the reaction mixture was concentrated
- dissolutionThe residue was dissolved in ethyl acetate
- washwashed with brine
- dry with materialThe organic layer was dried over MgSO4
- concentrationconcentrated in vacuo
- customto give the product
출처 및 근거
- ORD 기록
- ord-a95824d141a64b4eb3367fc72a420a56
- 출처 데이터셋
- uspto-grants-2014_05
- 특허 번호
- US08716293B2
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