Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 18472360 | HCID 18472360 | — |
| Reactant | HCID 178418435 | HCID 178418435 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 18472249 | HCID 18472249 | 69.7% |
Reaction Steps
In methanol (40ml) was dissolved N-(4-(1-methyl-piperidin-2-ylcarbonyl)-phenyl)-7-(4-methylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide (0.1g) under ice-cooling, and to the mixture was added sodium boron hydride (10mg). The mixture was stirred for 15 minutes, and to the mixture was added water. The mixture was concentrated and extracted with ethyl acetate. The organic layer was washed with water and saturated sodium chloride solution, and dried with anhydrous magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the residue was purified with silica gel column (ethyl acetate/methanol/triethylamine) to give crude crystals, which were recrystallized from ethanol-ethyl acetate-hexane to give N-(4-(hydroxy(1-methylpiperidin-2-yl)methyl)-phenyl)-7-(4-methylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide (Compound 158) (0.07g) as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06172061B2 |
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| Source dataset | uspto-grants-2001_01 |
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| ORD ID | ord-d431521f70f04bf89e8ec937c783bc66 |
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| Source note | uspto-grants-2001_01 |
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