HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 2-Chloro-5-nitro-3-(trifluoromethyl)pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | Phosphorus pentachloride | HCID 24819 | — |
| Reactant | HCID 178526837 | HCID 178526837 | — |
| Product | 2-Chloro-5-nitro-3-(trifluoromethyl)pyridine | HCID 3849140 | — |
Reaction Steps
A mixture of EXAMPLE 288A (1.69 g), phosphorus pentachloride (2.03 g), and phosphoryl trichloride (0.97 mL) was heated at 90° C. for 3 hours. After cooling, the reaction mixture was poured into ice, and extracted with ethyl acetate three times. The extract was washed with brine, dried over MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel eluting with 10% ethyl acetate in hexanes to provide the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09034875B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-ec164872dcac4fb09cc72f4871b86b4f |
| Source note | uspto-grants-2015_05 |