HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phenol, 4-amino-2-fluoro- → 4-(4-Amino-2-fluorophenoxy)-3-chloropicolinamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phenol, 4-amino-2-fluoro- | HCID 2735918 | — |
| Reactant | 3,4-Dichloropyridine-2-carboxamide | HCID 23165143 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-(4-Amino-2-fluorophenoxy)-3-chloropicolinamide | HCID 25231975 | 54.4% |
Reaction Steps
To a solution of 4-amino-2-fluorophenol (254 mg, 2.0 mmol) in DMF (5 mL) was added t-BuOK (359 mg, 3.2 mmol). The mixture was stirred at rt for 30 minutes. 3,4-dichloropicolinamide (420 mg, 2.2 mmol) was then added, and the mixture was microwaved at 120° C. for 2 hours. The mixture was cooled to rt, quenched with 25 mL of water. The resulted solution was extracted with EtOAc (30 mL×3) and the combined organic phases were washed with brine (30 mL×3), dried over Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (EtOAc/PE (v/v)=2/1) to give the title compound as a pale yellow solid (306 mg, 54.4%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09326975B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-d415ea83376e43ffa6ec1fe2bf97f52f |
| Source note | uspto-grants-2016_05 |