Methanol → Methyl 6-oxo-1,6-dihydropyridine-2-carboxylate
반응식
[O:1]=[C:2]1[NH:7][C:6]([C:8]([OH:10])=[O:9])=[CH:5][CH:4]=[CH:3]1.OS(O)(=O)=O.[CH3:16]O>>[O:1]=[C:2]1[NH:7][C:6]([C:8]([O:10][CH3:16])=[O:9])=[CH:5][CH:4]=[CH:3]1참가 물질
4
실험 절차
A mixture of commercially available 6-oxo-1,6-dihydropyridine-2-carboxylic acid (4.000 g; 28.75 mmol) and concentrated H2SO4 (3.5 ml) in anh. MeOH (65 ml) was refluxed, under nitrogen, for 22 h. MeOH was removed under reduced pressure, and the residue was basified by addition of a solution of 10% aq. NaHCO3. The mixture was then extracted with DCM (3×), and the mixed organic layers were dried over anh. MgSO4, filtered, and concentrated to dryness under reduced pressure affording methyl 6-oxo-1,6-dihydropyridine-2-carboxylate as a beige solid. LC-MS (conditions D): tR=0.54 min.; no ionisation.
후처리
- temperaturewas refluxed, under nitrogen, for 22 h
- customMeOH was removed under reduced pressure
- additionthe residue was basified by addition of a solution of 10% aq. NaHCO3
- extractionThe mixture was then extracted with DCM (3×)
- dry with materialthe mixed organic layers were dried over anh. MgSO4
- filtrationfiltered
- concentrationconcentrated to dryness under reduced pressure
출처 및 근거
- ORD 기록
- ord-74ac2210d9c842f5b2ff7b4c6e0a91f4
- 출처 데이터셋
- uspto-grants-2016_01
- 특허 번호
- US09242970B2
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