HuagongsheHuagongshe Chemistry Print Report · For research reference only
m-Chloroperbenzoic acid → HCID 67976751, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Reactant | HCID 67974202 | HCID 67974202 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67976751 | HCID 67976751 | 79.1% |
Reaction Steps
To a solution of 5-bromo-3-chloro-2,4-dimethylpyridine (441 mg; 2.0001 mmol) in dichloromethane (10 mL; 156.0 mmol) was added 3-chloroperoxybenzoic acid (70%, 0.5547 g; 2.250 mmol). The reaction mixture was stirred at room temperature for 3 hours. The reaction mixture was diluted with additional dichloromethane (100 mL), washed with saturated sodium bicarbonate, dried over magnesium sulfate, filtered, and evaporated in vacuo. The crude product was purified via flash chromatography on silica gel (40 g silica, solvent gradient: 0-100% ethyl acetate in dichloromethane) to yield 374.1 mg (79%) of the title compound. LCMS (ESI): M+H=236.2; 1H NMR (400 MHz, DMSO) δ 8.65 (s, 1H), 2.47 (s, 3H), 2.43 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08623889B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-3eb0fce377704c3fa6a6903c2a1dded7 |
| Source note | uspto-grants-2014_01 |