反応 #2146704

反応方程式

sulfuric acid

nitric acid

2-bromo-3-methoxypyridine

→

2-bromo-3-methoxy-6-nitropyridine

反応条件

後処理

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
   温度After the reaction solution was cooled down
4. 4
   workup.ADDITIONthe reaction solution was poured little by little
5. 5
   その他onto crushed ice
6. 6
   その他to generate precipitates
7. 7
   ろ過The precipitates were filtered
8. 8
   洗浄washed with water
9. 9
   その他The precipitates obtained
10. 10
    乾燥was dried over phosphorus pentaoxide under reduced pressure

実験手順

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).

出典