Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Reactant | HCID 11166749 | HCID 11166749 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 3013410 | HCID 3013410 | 59.9% |
Reaction Steps
To a solution of N-[4—(2-pyridylmethyl)phenyl]-7—(4-methylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide (200 mg) in tetrahydrofuran (10 ml) was added 3-chloro-perbenzoic acid (70%, 0.18 g) at 0° C., and the mixture was stirred at room temperature for 17 hours. To the reaction mixture was added sodium thio-sulfate solution, and the mixture was stirred for a few minutes. The mixture was extracted with ethyl acetate. The organic layer was washed with saturated sodium bicarbonate solution and saturated sodium chloride solution, dried with magnesium sulfate and concentrated to give crystals, which were collected by filtration and was recrystallized from ethanol to give N-[4—(1-oxidopyridin-2-ylmethyl)phenyl]-7—(4-methylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide (Compound 162) (124 mg) as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06413947B1 |
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| Source dataset | uspto-grants-2002_07 |
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| ORD ID | ord-60555d2ef5a84b038426e07f3461f0c7 |
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| Source note | uspto-grants-2002_07 |
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