Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylsilane | HCID 12052 | — |
| Reactant | HCID 23114188 | HCID 23114188 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 23114377 | HCID 23114377 | 81.7% |
Reaction Steps
To a solution of N-(3-hydroxy-2,2,6,7-tetramethyl-3-(2-methylphenyl)-2,3-dihydro-1-benzofuran-5-yl)-3,3-dimethylbutanamide (120 mg, 0.3 mmol) obtained in Example 242 in trifluoroacetic acid (2 mL) was added triethylsilane (71 mg, 0.6 mmol) under ice-cooling, and the mixture was stirred at room temperature for 1 hour. The reaction solution was added to water and the product was extracted with ethyl acetate. The organic layer was washed with an aqueous 1 N sodium hydroxide solution, water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:2) and recrystallized from ethyl acetate-hexane to obtain 93 mg (yield: 79%) of the title compound. Melting point: 161-162° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07465815B2 |
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| Source dataset | uspto-grants-2008_12 |
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| ORD ID | ord-1077b185812a4f25ad947fc5c1d7ec93 |
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| Source note | uspto-grants-2008_12 |
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