Reaktion #65752
ord-133574a6edea4a3e8e8cf537230a23b2
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.ADDITIONwas added dropwise to the solution
- 2workup.WAITleft
- 3Sonstigestanding in a refrigerator overnight
- 4FiltrationThe resulting crystals were collected by filtration
- 5SonstigeThe crystals were recrystallized from ethyl acetate
- 6Sonstigeto give colorless plates
Vorschrift
In 90 ml of 2% hydrochloric acid was dissolved 2.52 g (10 mmol) of 2-amino-3,4-diethoxycarbonyl-6-methylpyridine. A solution of 0.83 g (1.2 eq.) of sodium nitrite dissolved in 3 ml of water was added dropwise to the solution. The mixture was stirred at room temperature for 1 hour and left standing in a refrigerator overnight. The resulting crystals were collected by filtration. The crystals were recrystallized from ethyl acetate to give colorless plates.