HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,4-Dimethylpyridine → 3,4-Dimethylpyridine 1-oxide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,4-Dimethylpyridine | HCID 11417 | — |
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3,4-Dimethylpyridine 1-oxide | HCID 302454 | 61.1% |
Reaction Steps
To a solution of 3,4-dimethylpyridine (100.0 g, 0.93 mol) in dichloromethane was added m-CPBA (320.0 g, 1.87 mol) at the room temperature. The reaction mixture was stirred at room temperature overnight, and then quenched with saturated solution of Na2S2O3 (100 mL). The organic layer was separated and the aqueous phase was extracted with CH2Cl2 (300 mL×3). The combined organic layers were dried over anhydrous Na2SO4, filtered and evaporated under vacuum to yield a residue that was purified by column chromatography on silica gel (10-100% MeOH in EtOAc) to give 3,4-dimethylpyridine 1-oxide (70.0 g, 61%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08969386B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-2c3e9c84d5274d16aad9c3416c7d3d69 |
| Source note | uspto-grants-2015_03 |