HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 1-[3-(4-Bromo-2-fluorophenyl)prop-2-ynyl]piperidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 1-(Prop-2-yn-1-yl)piperidine | HCID 336652 | — |
| Reactant | 4-Bromo-2-fluoro-1-iodobenzene | HCID 2724516 | — |
| Catalyst | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| Catalyst | HCID 178418476 | HCID 178418476 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 1-[3-(4-Bromo-2-fluorophenyl)prop-2-ynyl]piperidine | HCID 23087565 | 44.7% |
Reaction Steps
To a solution of 1-bromo-3-fluoro-4-iodobenzene (2.5 g), 1-prop-2-ynylpiperidine (1.5 g), dichlorobis(triphenylphosphine)palladium(II) (300 mg) and copper(I) iodide (40 mg) in N,N-dimethylformamide (20 ml) was added triethylamine (10 ml) under a nitrogen atmosphere, and the solution was stirred for 1.5 hours at room temperature. A saturated aqueous solution of ammonium chloride was added thereto followed by stirring, the solution was extracted with ethyl acetate, then sequentially washed with water and brine, and 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 (1.1 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07612114B2 |
| Source dataset | uspto-grants-2009_11 |
| ORD ID | ord-a27f7648638f46efbd014ddcadea7c91 |
| Source note | uspto-grants-2009_11 |