HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cyclohexanol → 3-Fluoro-5-cyclohexyloxybenzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cyclohexanol | HCID 7966 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 3,5-Difluorobenzonitrile | HCID 587204 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 3-Fluoro-5-cyclohexyloxybenzonitrile | HCID 59553135 | — |
Reaction Steps
Sodium hydride (1.92 g, 48.0 mmol) is slowly added to a stirred solution of cyclohexanol (4.01 g, 40.0 mmol) in DMF (30 ml) at 0-5° C. under nitrogen. After 2.5 hours, 3,5-difluorobenzonitrile (5.56 g, 40.0 mmol) is slowly added over 5 min. The mixture is allowed to warm to room temperature and stirred for an additional 12 hours. The mixture is diluted with ether (150 ml), washed with water, brine (30 ml), dried over Na2SO4 and evaporated. The residue is purified by column chromatography on silica gel eluting with ethyl acetate:hexanes (1:10) to provide 3-fluoro-5-cyclohexyloxybenzonitrile as a yellow oil. MS: 220 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07829560B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-4a413aa47ff34cd4b7be25fdc592d69b |
| Source note | uspto-grants-2010_11 |