HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Iodide → 1-[2-(4-Bromophenoxy)ethyl]azepane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | 4-Bromophenol | HCID 7808 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | N-(2-chloroethyl)perhydroazepine hydrochloride | HCID 24188283 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 1-[2-(4-Bromophenoxy)ethyl]azepane | HCID 13063544 | 96.7% |
Reaction Steps
To a suspension of 60% sodium hydride (1.6 g) in N,N-dimethylformamide (50 ml) was added 4-bromophenol (3.0 g) under a nitrogen atmosphere, the solution was stirred for 10 minutes at room temperature, then 1-(2-chloroethyl)azepane hydrochloride (4.0 g) and sodium iodide (in catalytic amounts) were sequentially added thereto followed by stirring overnight at 80° C. Water was added thereto followed by stirring, the solution was extracted with ethyl acetate, then sequentially washed with water and brine, and 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 (5.0 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07612114B2 |
| Source dataset | uspto-grants-2009_11 |
| ORD ID | ord-8e829b19eca74fc380721aae8418448c |
| Source note | uspto-grants-2009_11 |