Nitric Acid → 2-Nitro-1-oxo-1lambda~5~-pyridine
Reaktionsgleichung
OS(O)(=O)=O.C[C:7]1[C:12](C)=[CH:11][CH:10]=[CH:9][N+:8]=1[O-:14].C([O-])([O-])=O.[Na+].[Na+].[N+:21]([O-])([OH:23])=[O:22]>>[N+:21]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][N+:8]=1[O-:14])([O-:23])=[O:22]Komponenten
Versuchsvorschrift
To 400 mL of concentrated H2SO4 was added slowly 130 g of impure 2,3-dimethylpyridine N-oxide. Fuming HNO3 (330 mL) was slowly added at a rate to keep the temperature between 120° C. and 170° C. After addition was complete, the temperature was held at 103° C. for 3 hours and then the reaction was cooled. The crude reaction was added to 1 kg ice in a large pan, then, with stirring, 1.1 kg Na2CO3 was added. After cooling to room temperature, the solids were removed by suction filtration from the solution. The filtrate was extracted with chloroform. The solids were washed with hot chloroform (3 times). The combined reduced organic extracts yielded 110 g of the crude desired nitropyridine N-oxide as an orange solid. ##STR8## 4-acetylamino-2,3-dimethylpyridine
Aufarbeitung
- customthe temperature between 120° C. and 170° C
- additionAfter addition
- temperaturethe reaction was cooled
- customThe crude reaction
- customthe solids were removed by suction filtration from the solution
- extractionThe filtrate was extracted with chloroform
- washThe solids were washed with hot chloroform (3 times)
Quellen und Nachweise
- ORD-Eintrag
- ord-2296f44a8546406794a00abe14060185
- Quelldatensatz
- uspto-grants-1995_07
- Patentnummer
- US05430007
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