Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 68429387 | HCID 68429387 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ether tetrahydrofuran | HCID 21868444 | — |
| Product | HCID 68429508 | HCID 68429508 | 50% |
Reaction Steps
To a mixture of lithium aluminum hydride (0.066 g) and THF-diethyl ether (2 mL-10 mL) was added the compound obtained in step 2 (0.40 g), and the resulting mixture was stirred at room temperature for 3 hr under a nitrogen atmosphere. Lithium aluminum hydride (0.066 g) was added again, and the resulting mixture was stirred at room temperature for 2 hr under a nitrogen atmosphere. 1N Aqueous sodium hydroxide solution (0.13 mL), saturated aqueous ammonium chloride (0.13 mL) and water (0.13 mL) were added, and the resulting mixture was stirred at room temperature for 4 hr. The precipitate was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (solvent gradient; 0→40% ethyl acetate/hexane) to give 4-benzyl-8-phenoxy-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine (0.19 g, 50%) as a white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08329687B2 |
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| Source dataset | uspto-grants-2012_12 |
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| ORD ID | ord-0a3a740dc5604adc97e4368d1752d5eb |
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| Source note | uspto-grants-2012_12 |
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