HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → HCID 117899759, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | 1,5-Dibromopentane | HCID 8100 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 117899711 | HCID 117899711 | — |
| Catalyst | Tetrabutylammonium Bromide | HCID 74236 | — |
| Solvent | Ethyl acetate hexane | HCID 21226206 | — |
| Product | HCID 117899759 | HCID 117899759 | 89.2% |
Reaction Steps
To 60 ml of acetonitrile were added 3.0 g (11.5 mmol) of 4-chloro-2-fluoro-5-(2,2,2-trifluoroethylthio)phenol, 13.2 g (57.4 mmol) of 1,5-dibromopentane, 2.1 g (15.0 mmol) of potassium carbonate and 0.37 g (1.15 mmol) of tetra-n-butylammonium bromide. The mixture was refluxed for 1.5 hour under heating. The mixture was allowed to cool to room temperature, and insoluble matters were removed by filtration. Then the filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (developing solvent: a mixed solvent of n-hexane ethyl acetate=20:1), to obtain 4.2 g (yield: 89%) of an intended product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09332754B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-cc84f46bf7f14dcb9b50afc2f539d3a3 |
| Source note | uspto-grants-2016_05 |