HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 1-[2-(5-Bromopyridin-2-yloxy)ethyl]azepane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2,5-Dibromopyridine | HCID 69353 | — |
| Reactant | Hexahydro-1H-azepine-1-ethanol | HCID 88615 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 1-[2-(5-Bromopyridin-2-yloxy)ethyl]azepane | HCID 57934072 | 96.1% |
Reaction Steps
To a solution of 2-azepan-1-ylethanol (5.0 g) in N,N-dimethylformamide (100 ml) was added 60% sodium hydride (1.5 g) under a nitrogen atmosphere, the solution was stirred for 1 hour at room temperature, 2,5-dibromopyridine (7.5 g) was then added thereto followed by stirring for 4.5 hours at room temperature. Water was added thereto followed by stirring, the solution was extracted with ethyl acetate, then sequentially washed with water and brine, dried over anhydrous magnesium sulfate, and then the solvent was evaporated in vacuo. The residue was purified by NH silica gel column chromatography (hexane-ethyl acetate system) to provide the title compound (9.1 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07960412B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-9fdb6ba9638249f79ab7692255992852 |
| Source note | uspto-grants-2011_06 |