HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium peroxymonosulphate → 4-[(4-Fluorophenyl)ethynyl]benzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium peroxymonosulphate | HCID 10313463 | — |
| Reactant | 4-[2-(4-Fluorophenyl)ethynyl]benzaldehyde | HCID 45490114 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-[(4-Fluorophenyl)ethynyl]benzoic acid | HCID 22628857 | 94% |
Reaction Steps
To a solution of 4-[(4-fluorophenyl)ethynyl]benzaldehyde (10.39 g; 46.37 mmol, intermediate which may be obtained according to methods disclosed in EP03 103780.7) in DMF (400 mL) was added potassium peroxomonosulfate (28.5 g, 46.4 mmol) in one portion at rt. The reaction mixture was stirred at rt overnight. The reaction mixture was poured in water (2 L) and the resulting precipitate was filtered off, washed with water and dried under reduced pressure to give 10.45 g (94%) of the title compound as a white powder. HPLC, Rt: 3.98 min (purity: 98.6%). 1H NMR (DMSO-d6) δ: 13.15 (brs, 1H), 7.96 (d, J=8.1 Hz, 2H), 7.64 (m, 4H), 7.29 (t, J=8.9 Hz, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07947851B2 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-45dc4f89ac30406f97bc289cace16dce |
| Source note | uspto-grants-2011_05 |