Nitric Acid → 2,6-Dichloro-3-nitropyridine

Temperature

50 °C

2,6-Dichloropyridine, 25.0 gm (0.168 mole) was added slowly under constant stirring to concentrated sulfuric acid at 20°–25° C. To this solution, 75.0 gm of concentrated nitric acid (98.0%) was added slowly, keeping the reaction temperature below 50° C. After the addition, the resulting mixture was heated to 100°–105° C. for 5.0 hrs. The progress of the reaction was monitored by TLC. After the reaction was over, the reaction mixture was cooled to 50° C. and poured in ice water. The resulting precipitate was filtered and washed with water. The wet cake thus obtained was dried to give 24.5 gm of 2,6-dichloro-3-nitropyridine. The yield of 2,6-dichloro-3-nitropyridine was 75.38% and the GC purity was 99.5%.

1. customthe reaction temperature below 50° C
2. additionAfter the addition
3. temperaturethe resulting mixture was heated to 100°–105° C. for 5.0 hrs
4. filtrationThe resulting precipitate was filtered
5. washwashed with water
6. customThe wet cake thus obtained
7. customwas dried

ORD record

ord-6b0673b7c0f7461ea56137bf6adfbc1b

Source dataset

uspto-grants-2007_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07256295B2