HuagongsheHuagongshe Chemistry Print Report · For research reference only
m-Chloroperbenzoic acid → HCID 54150072, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Reactant | HCID 19895597 | HCID 19895597 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 54150072 | HCID 54150072 | 7.3% |
Reaction Steps
261 mg of 6-acetyl-3,4-dihydro-2,2 -dimethyl-4-(2-pyridyl)-2H-1-benzopyran were dissolved in 20 ml of dichloromethane at room temperature and 250 mg of m-chloroperbenzoic acid were added. After stirring at room temperature for 3 days the mixture was washed in succession with sodium bisulphite solution, sodium bicarbonate solution and water, dried over sodium sulphate and evaporated. The residue was chromatographed on silica gel using 2%-5% (v/v) methanol/chloroform for the elution. The resulting foam was triturated with methylcyclohexane and the solid obtained was recrystallized from t-butyl methyl ether to give 20 mg of 2-(6-acetyl-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran-4-yl)pyridine N-oxide of melting point 132°-133° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05118694 |
| Source dataset | uspto-grants-1992_06 |
| ORD ID | ord-7cfd0731a5544e0698089f8758cff210 |
| Source note | uspto-grants-1992_06 |