HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 86634744, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Pyridine, 2,4,6-trichloro- | HCID 27665 | — |
| Reactant | 2,6-Difluorophenol | HCID 94392 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86634744 | HCID 86634744 | — |
Reaction Steps
2,6-Difluorophenol (10.0 mmol) is added to a mixture of sodium hydride (240 mg, 10 mmol) in DMF (6 mL). The reaction mixture is stirred for 30 minutes at room temperature. The reaction mixture is cooled to 0° C., and 2,4,6-trichloropyridine is added. The reaction mixture is stirred at 0° C. for 1 hour, then at room temperature for 4 hours. The reaction mixture is partitioned between ethyl acetate and water, the organic layer is washed with 2N NaOH, water, brine, dried, and concentrated. The residue is purified via chromatography eluting with 5:1 hexane:ethyl acetate to afford 2,6-dichloro-4-(2,6-difluorophenoxy)pyridine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08022222B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-ab9821b7930a4840ab779b1a13f174d5 |
| Source note | uspto-grants-2011_09 |