HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2,4,6-Trichloro-3-nitropyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2,6-Dichloro-3-nitropyridin-4-amine | HCID 282740 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Product | 2,4,6-Trichloro-3-nitropyridine | HCID 12275766 | 80.7% |
Reaction Conditions
| Temperature | 2.5 °C |
|---|
Reaction Steps
2,6-dichloro-3-nitropyridine-4-amine (2.27 g, 10.9 mmol) was added to 48 mL concentrated hydrochloric acid, and cooled to 0-5° C. To the solution was added sodium nitrite (2.26 g, 32.7 mmol) in batches. After the addition of sodium nitrite, the reaction solution was stirred for 1 h at 0-5° C., and then stirred for 2 h at 25° C., adjusted to pH=7 with 40% sodium hydroxide solution, and extracted with ethyl ether. After the organic phase was dried (Na2SO4) and concentrated, it was subjected to column chromatography eluted with petroleum ether to afford 2 g white solid with a yield of 80.7%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08680089B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-60852630ef314bbdb85be5cbac232f7d |
| Source note | uspto-grants-2014_03 |