HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 1-(3-bromophenyl)-2-[1-(2,2,2-trifluoroethyl)-1H-pyrazol-4-yl]ethane-1,2-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Reactant | Potassium Permanganate | HCID 516875 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 4-[(3-bromophenyl)ethynyl]-1-(2,2,2-trifluoroethyl)-1H-pyrazole | HCID 59772730 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | 1-(3-bromophenyl)-2-[1-(2,2,2-trifluoroethyl)-1H-pyrazol-4-yl]ethane-1,2-dione | HCID 59772691 | 82% |
Reaction Steps
To a solution of 4-[(3-bromophenyl)ethynyl]-1-(2,2,2-trifluoroethyl)-1H-pyrazole (4.90 g, 14.9 mmol) in acetone (150 mL) is added a warm (˜40° C.) solution of NaHCO3 (0.75 g, 8.9 mmol) and MgSO4 (2.70 g, 22.4 mmol) in H2O (150 mL) followed by the addition of solid potassium permanganate (5.2 g, 32.8 mmol) in one portion. After stirring for 40 minutes at room temperature, the reaction mixture is extracted with a solution of Et2O/hexane (1/1) until no product left in aqueous layer. The combined organic extracts is dried (MgSO4) and concentrated to dryness to afford the title compound (4.4 g, 82%) as a solid. mp: 66-67° C. MS (−) ES: 359 (M−H)−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07705030B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-05190f0c846c4fe6be16edb35008c42f |
| Source note | uspto-grants-2010_04 |