HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 2-Chloro-4-(2-chloro-4-difluoromethoxy-phenyl)-3-nitro-2,3-dihydro-pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 4-(2-chloro-4-difluoromethoxy-phenyl)3-nitro-3H-pyridin-2-one | HCID 22052138 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2-Chloro-4-(2-chloro-4-difluoromethoxy-phenyl)-3-nitro-2,3-dihydro-pyridine | HCID 22052084 | 96% |
Reaction Steps
To 10 mL of POCl3 was added 4-(2-chloro-4-difluoromethoxy-phenyl)3-nitro-3H-pyridin-2-one (0.20 g, 0.63 mmol), followed by the addition of DMF (1–2 mL) and the reaction refluxed overnight. The reaction mixture was cooled to room temperature and poured over ice/H2O (200 mL). The solution was extracted with EtOAc, washed H2O, brine, dried Na2SO4, filtered, and concentrated in vacuo to give 0.176 g (96%) of 2-chloro-4-(2-chloro-4-difluoromethoxy-phenyl)-3-nitro-2,3-dihydro-pyridine as brown viscous oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07067658B2 |
| Source dataset | uspto-grants-2006_06 |
| ORD ID | ord-e2e66cbba6904a6cbefe7273563f8970 |
| Source note | uspto-grants-2006_06 |