HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 2-(2,2-bisfluoromethyl-6-iodo-2H-1-benzopyran-4-yl)pyridine N-oxide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Reactant | 2,2-bisfluoromethyl-6-iodo-4-(2-pyridyl)-2H-1-benzopyran | HCID 21831344 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-(2,2-bisfluoromethyl-6-iodo-2H-1-benzopyran-4-yl)pyridine N-oxide | HCID 70285558 | 23.1% |
Reaction Steps
To a mixture of 1.04 g of 2,2-bisfluoromethyl-6-iodo-4-(2-pyridyl)-2H-1-benzopyran and 20 ml of methylene chloride was added 0.78 g of m-chloroperbenzoic acid (70%) with stirring under ice-cooling. The mixture was stirred under ice-cooling for 1 hour and then stirred at room temperature for 25 hours. Potassium carbonate solution was added thereto and the mixture was extracted with methylene chloride. The organic layer was washed with water and dried. The solvent was distilled off and the resultant residue was purified using silica gel column chromatography (developing solution, MeOH:CH2Cl2 =1:99) to obtain 0.25 g of oily 2-(2,2-bisfluoromethyl-6-iodo-2H-1-benzopyran-4-yl)pyridine N-oxide represented by the following formula.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05977167 |
| Source dataset | uspto-grants-1999_11 |
| ORD ID | ord-87669ddd19974389a28aa5f68ab09414 |
| Source note | uspto-grants-1999_11 |