Methanol → Methyl 6-bromo-2,3-difluorobenzoate
反応式
[Br:1][C:2]1[C:7]([C:8]([OH:10])=[O:9])=[C:6]([F:11])[C:5]([F:12])=[CH:4][CH:3]=1.OS(O)(=O)=O.[CH3:18]O>>[Br:1][C:2]1[C:7]([C:8]([O:10][CH3:18])=[O:9])=[C:6]([F:11])[C:5]([F:12])=[CH:4][CH:3]=1参加物
4
実験手順
A stirred solution of 6-bromo-2,3-difluorobenzoic acid and conc. H2SO4 in MeOH was heated at reflux for 18 h. The reaction mixture was cooled to rt and concentrated under reduced pressure. To the residue was carefully added a satd. aq. NaHCO3 solution. The resulting mixture was extracted with CH2Cl2. The combined extracts were dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The residue obtained was dried under high vacuum to afford the title compound. ESI MS (M+H) 251.
後処理
- temperatureat reflux for 18 h
- concentrationconcentrated under reduced pressure
- additionTo the residue was carefully added a satd
- extractionThe resulting mixture was extracted with CH2Cl2
- dry with materialThe combined extracts were dried over anhydrous Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe residue obtained
- customwas dried under high vacuum
出典と根拠
- ORDレコード
- ord-f4c71742eea44a02906d33f912a0a436
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09440982B2
反応ノート
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