Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 4-(3-Phenylpropyl)pyridine N-oxide | HCID 688320 | — |
| Reactant | 6-Ethyl-2,2-dimethyl-2h-chromene | HCID 14743502 | — |
| Reactant | Sodium Hypochlorite | HCID 23665760 | — |
| Product | HCID 11658499 | HCID 11658499 | 69% |
Reaction Steps
To a solution (2 mL) of ethyl acetate containing 100 mg (0.53 mmol) of 6-ethyl-2,2-dimethyl-2H-1-benzopyran (synthesized according to the method described in Jananese Patent Application Laid-open No. Sho 62-273972), salen manganese complex (17 mg, 0.016 mmol), 4-(3-phenylpropyl)-pyridineoxide) (12 mg, 0.053 mmol) and aqueous sodium hypochlorite solution (0.96 g, 1.14 Kg/mol, 1.1 mmol) were added at room temperature, and stirred for two hours at room temperature. After Celite filtration upon addition of water, organic phase was separated, washed with aqueous saturated sodium chloride solution, and dried over anhydride sodium sulfate. After distilling off the solvent, the residue was purified by silica gel column chromatography (chloroform) to obtain 75 mg of the intended compound in brown oily substance (Yield 69%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07041700B2 |
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| Source dataset | uspto-grants-2006_05 |
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| ORD ID | ord-ce30db6c705a4f6abcaa31d3b95f84cf |
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| Source note | uspto-grants-2006_05 |
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