HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 22320244, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 22320133 | HCID 22320133 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22320244 | HCID 22320244 | 57% |
Reaction Steps
A solution of 4,5-difluoro-2-[[1-(2-pyridinyl)-1H-pyrazol-5-yl]amino]benzoic acid (7.00 g, 22.1 mmol) in phosphorous oxychloride (10.3 mL, 111 mmol) was heated under reflux for 1 hour. The solution was allowed to cool to room temperature, and poured into iced water. After neutralization by addition of a sodium hydroxide solution, the organic matter was extracted with chloroform. The extract was washed with saturated brine and water, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue thus obtained was purified by silica gel column chromatography (chloroform) to give the title compound (3.99 g, 57% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06949648B2 |
| Source dataset | uspto-grants-2005_09 |
| ORD ID | ord-1a5c8b76eba04303aad7d51726d38a22 |
| Source note | uspto-grants-2005_09 |