反应 #2146684

反应方程式

sulfuric acid

nitric acid

2-bromo-3-methoxypyridine

→

2-bromo-3-methoxy-6-nitropyridine

反应条件

后处理

1. 1
   workup.STIRRINGthe mixture was stirred at room temperature for 30 minutes
2. 2
   workup.STIRRINGfurther stirred for 1.5 hours
3. 3
   温度After the reaction solution was cooled to room temperature
4. 4
   workup.ADDITIONthe reaction solution was poured little by little
5. 5
   其他into crushed ice
6. 6
   其他to generate precipitates
7. 7
   过滤The precipitates were filtered
8. 8
   洗涤washed with water
9. 9
   干燥dried over phosphorus pentaoxide under reduced pressure

实验过程

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).

来源