Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | Ethanol | HCID 702 | — |
| Reactant | HCID 59485055 | HCID 59485055 | — |
| Catalyst | HCID 178418390 | HCID 178418390 | — |
| Product | HCID 59485010 | HCID 59485010 | 49% |
Reaction Steps
To a solution of ethanol (7.0 mL) containing 1-{2-[(benzyloxy)methyl]-2,4,6,7-tetramethyl-2,3-dihydro-1-benzofuran-5-yl}-4-(4-methoxyphenyl)piperazine (30 mg, 0.0628 mmol) synthesized in Example 134, 10% palladium carbon (500 mg) and formic acid (7.0 mL) were serially added, and the mixture was stirred at 100° C. for 15 hours. After cooled to room temperature, palladium carbon was removed by filtration, and the solvent was removed under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate 97:3-80:20) and crystallized from ethyl acetate-hexane to obtain 290 mg of the title compound (yield: 49%). Melting point was 120 to 124° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08288390B2 |
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| Source dataset | uspto-grants-2012_10 |
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| ORD ID | ord-0fb84a30801b41c2a72766ef97c85c93 |
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| Source note | uspto-grants-2012_10 |
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