Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 68967526 | HCID 68967526 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86730316 | HCID 86730316 | 58% |
Reaction Steps
1-Benzyl-4-(4-(4,4-dimethyl-4,5-dihydrooxazol-2-yl)phenyl)piperidin-4-ol described in Production Example 7-1 (13.4 g, 36.8 mmol) was dissolved in ethanol (300 mL), then sulfuric acid was added, and the mixture was stirred at 90° C. for 12 hours. The reaction mixture was cooled to room temperature and then the solvent was evaporated under vacuum. The resultant residue was dissolved in dichloromethane, the resultant was washed with a saturated aqueous sodium bicarbonate solution, and then the organic layer was dried over anhydrous sodium sulfate and filtered. The solvent was evaporated under vacuum and the resultant residue was purified with NH silica gel column chromatography (n-heptane:ethyl acetate=4:1-1:1). The target fraction was concentrated under vacuum to obtain the title compound (7.23 g, 58%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08933099B2 |
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| Source dataset | uspto-grants-2015_01 |
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| ORD ID | ord-b9d8680da755463ca73df4ff1b6dd3eb |
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| Source note | uspto-grants-2015_01 |
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