Nitric Acid → 2-Bromo-3-methoxy-6-nitropyridine

Temperature

55 °C

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).

1. stirringthe mixture was stirred at room temperature for 30 minutes
2. stirringthe mixture was stirred for 1.5 hours
3. temperatureAfter the reaction solution was cooled down
4. additionthe reaction solution was poured little by little
5. customonto crushed ice
6. customto generate precipitates
7. filtrationThe precipitates were filtered
8. washwashed with water
9. customThe precipitates obtained
10. dry with materialwas dried over phosphorus pentaoxide under reduced pressure

ORD record

ord-df12d0973c42432f9218ffc903decdb4

Source dataset

uspto-grants-2012_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08277777B2