Reaktion #2146689

Reaktionsgleichung

sulfuric acid

nitric acid

2-bromo-3-methoxypyridine

→

2-bromo-3-methoxy-6-nitropyridine

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture was stirred at room temperature for 10 minutes
2. 2
   workup.STIRRINGfurther stirred for one hour
3. 3
   TemperaturAfter the reaction solution was cooled to room temperature
4. 4
   workup.ADDITIONthe reaction solution was poured little by little
5. 5
   Sonstigeinto crushed ice
6. 6
   Sonstigeto generate precipitates
7. 7
   FiltrationThe precipitates were filtered
8. 8
   Waschenwashed with water
9. 9
   Trocknendried over phosphorus pentaoxide under reduced pressure

Vorschrift

83 mL of conc. sulfuric acid was cooled down to −5° C., and 83 mL of 90% nitric acid was carefully added thereto. Subsequently, 20.69 g (corresponding to 110.04 mmol) of 2-bromo-3-methoxypyridine was carefully added thereto. After the reaction mixture was stirred in an ice bath for 5 minutes, the mixture was stirred at room temperature for 10 minutes, and then was heated to 55° C. and further stirred for one hour. After the reaction solution was cooled to room temperature, the reaction solution was poured little by little into crushed ice to generate precipitates. The precipitates were filtered and washed with water, and then dried over phosphorus pentaoxide under reduced pressure, to obtain 17.41 g (corresponding to 74.71 mmol) of 2-bromo-3-methoxy-6-nitropyridine (FIG. 3, Step 2).

Quelle