Ethanol → Ethyl 3-Aminoisonicotinate
Reaktionsgleichung
[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[C:8]([OH:10])=[O:9].S(=O)(=O)(O)O.[NH4+].[OH-].[CH2:18](O)[CH3:19]>>[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[C:8]([O:10][CH2:18][CH3:19])=[O:9]Komponenten
5
Versuchsvorschrift
To a solution of 1 g (7.25 mmol) of 3-amino-4-pyridinecarboxylic acid in 5 mL of ethyl alcohol was added 2 mL of sulfuric acid. The mixture was warmed under reflux for 2 h. It was cooled and basified with conc. NH4OH solution to pH=8. The resulting solution was extracted with ethyl acetate and the organic layer was washed with brine and water, dried (MgSO4) and concentrated in vacuo to give 1.04 g of the title compound as a white solid (87%).
Aufarbeitung
- temperatureThe mixture was warmed
- temperatureunder reflux for 2 h
- temperatureIt was cooled
- extractionThe resulting solution was extracted with ethyl acetate
- washthe organic layer was washed with brine and water
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-67d96eb2975649e3885db6bf1f096cfe
- Quelldatensatz
- uspto-grants-2009_07
- Patentnummer
- US07560564B2
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