Reaktion #2146684

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 30 minutes
2. 2
   workup.STIRRINGfurther stirred for 1.5 hours
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

262 mL of conc. sulfuric acid was cooled down to −2° C., and 262 mL of 90% nitric acid was carefully added thereto. Subsequently, 65.3 g (corresponding to 0.347 mmol) of 2-bromo-3-methoxypyridine was carefully added thereto. After the reaction mixture was stirred in an ice bath for 10 minutes, the mixture was stirred at room temperature for 30 minutes, and then was heated to 55° C. and further stirred for 1.5 hours. 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 55.7 g (corresponding to 0.239 mol) of 2-bromo-3-methoxy-6-nitropyridine (FIG. 2, Step 2).

Quelle