HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 2-Bromo-4-methyl-3-nitro-pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Phosphorus oxybromide | HCID 24613 | — |
| Reactant | 2-Hydroxy-4-methyl-3-nitropyridine | HCID 345370 | — |
| Solvent | 1,1-Dichloroethane | HCID 6365 | — |
| Product | 2-Bromo-4-methyl-3-nitro-pyridine | HCID 19926089 | 71.8% |
Reaction Steps
The 4-methyl-3-nitropyridin-2(1H)-one (110 g, 0.71 mol) was suspended in dichloroethane (1 L). The solution of phosphorus oxybromide (317 g, 1.1 mol) in dichloroethane (1 L) was added dropwise thereto at the ambient temperature. The reaction mixture was refluxed for 12 hours. The mixture was allowed to cool to room temperature, poured into ice water, and neutralized with potassium carbonate. The organic layer was separated, washed with water and brine, and dried over sodium sulfate. The solvent was evaporated to provide the title compound (yield 71.8%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09440968B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-ebac018909a54f20af991c206b66b15b |
| Source note | uspto-grants-2016_09 |