Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | (3-Bromopropyl)benzene | HCID 12503 | — |
| Reactant | Tert-butyl 1,4-diazepane-1-carboxylate | HCID 2756058 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 21994061 | HCID 21994061 | — |
Reaction Steps
To a solution of 4.50 g (22.47 mmol.) of 1-tert-butoxycarbonyl-2,3,5,6-tetrahydro-7H-1,4-diazepine in ethanol (50 ml) were added, at room temperature, 4.7 ml (33.72 mmol.) of triethylamine and 4.47 g (22.45 mmol.) of 1-bromo-3-phenylpropane. The mixture was heated under reflux for 8 hours under nitrogen atmosphere. To the reaction system were further added 4.7 ml (33.72 mmol.) of triethylamine and 4.47 g (22.45 mmol.) of 1-bromo-3-phenylpropane. The mixture was heated for 16 hours under reflux, which was cooled to room temperature. To the reaction system was added ethyl acetate, which was washed with water and a saturated aqueous saline solution, followed by drying over magnesium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by means of a column chromatography. The solvent was distilled off under reduced pressure to give the object compound as a yellow liquid product. The yield was 5.41 g (76%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06235731B1 |
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| Source dataset | uspto-grants-2001_05 |
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| ORD ID | ord-be9e4f1ac010422a8bd77a2783a151c2 |
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| Source note | uspto-grants-2001_05 |
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