HuagongsheHuagongshe Chemistry Print Report · For research reference only
Monobasic potassium phosphate → 4-Cyano-2,6-difluorobenzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Monobasic potassium phosphate | HCID 516951 | — |
| Reactant | 3,5-Difluoro-4-formylbenzonitrile | HCID 16218256 | — |
| Reactant | Sodium Chlorite | HCID 23668197 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Water | HCID 962 | — |
| Product | 4-Cyano-2,6-difluorobenzoic acid | HCID 44557933 | 99.3% |
Reaction Steps
To a solution of 3,5-difluoro-4-formylbenzonitrile (0.2 g, 1.1 mmol) in dimethylsulfoxide (10 mL), were added a aqueous solution of potassium dihydrogen phosphate (0.41 g, 2.9 mmol in 0.4 mL of water), sodium chlorite (0.216 g, 2.3 mmol in 4 mL of water) in one lot at an ambient temperature. The resulting reaction mixture was stirred for about 1 hour. The reaction mass was diluted with water (100 mL). The aqueous phase was extracted with ethyl acetate (3×100 mL). The combined organic layer dried over anhydrous sodium sulfate, filtered and concentrated to afford 4-cyano-2,6-difluorobenzoic acid (200 mg, 91.32%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09364466B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-1ea0b0968f1f456b889704c080771dc1 |
| Source note | uspto-grants-2016_06 |