Reaktion #2146704

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.STIRRINGthe mixture was stirred for 1.5 hours
3. 3
   TemperaturAfter the reaction solution was cooled down
4. 4
   workup.ADDITIONthe reaction solution was poured little by little
5. 5
   Sonstigeonto crushed ice
6. 6
   Sonstigeto generate precipitates
7. 7
   FiltrationThe precipitates were filtered
8. 8
   Waschenwashed with water
9. 9
   SonstigeThe precipitates obtained
10. 10
    Trocknenwas dried 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. Then, 65.3 g (corresponding to 0.347 mmol) of 2-bromo-3-methoxypyridine was carefully thereto. After the resulting mixture was stirred in an ice bath for 10 minutes, the mixture was stirred at room temperature for 30 minutes. Then, after the temperature of the mixture was raised up to 55° C., the mixture was stirred for 1.5 hours. After the reaction solution was cooled down, the reaction solution was poured little by little onto crushed ice to generate precipitates. The precipitates were filtered and washed with water. The precipitates obtained was 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. 1, Step 2).

Quelle