HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 2-Chloro-5,6-dimethylpyridine-3-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 5,6-Dimethyl-2-oxo-1,2-dihydropyridine-3-carbonitrile | HCID 590532 | — |
| Product | 2-Chloro-5,6-dimethylpyridine-3-carbonitrile | HCID 12891106 | 66.7% |
Reaction Steps
Phosphorus oxychloride (15 mL) was added to 2-oxo-1,2-dihydro-5,6-dimethyl pyridine-3-carbonitrile (2.00 g, 13.5 mmol) in a two neck 50 mL round bottom flask, and this mixture was stirred at RT for 1 h, and then refluxed for 12 h. Afterwards, the excess phosphorous oxychloride was distilled off, and the residue was poured into ice cooled water. The aqueous solution was basified with saturated sodium bicarbonate solution, and the precipitate that formed was filtered off to afford the title compound (1.50 g), yield: 66.7%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09040558B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-b309e95cbe9f4594af1d5931b4a3cb26 |
| Source note | uspto-grants-2015_05 |