HuagongsheHuagongshe Chemistry Print Report · For research reference only
Imidazole → 3-{[tert-Butyl(dimethyl)silyl]oxy}benzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | 3-Cyanophenol | HCID 13394 | — |
| Reactant | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 3-{[tert-Butyl(dimethyl)silyl]oxy}benzonitrile | HCID 22661489 | 92% |
Reaction Steps
To a solution of 3-cyanophenol (5 g, 42 mmol) and imidazole (6.3 g, 92 mmol) in N,N-dimethylformamide (85 mL) at 0° C. was added tert-butyldimethylsilylchloride (7.6 g, 50 mmol). After 10 min, the reaction was warmed to room temperature and stirred for 24 h. The solvent was removed under vacuum. The residual oil was diluted with water (100 mL) and extracted with ether (300 mL). The ether layer was back-extracted with water (3×100 mL) and brine (100 mL), dried (MgSO4) and filtered. Concentration and flash chromatography (silica, 50% ethyl acetate in petroleum ether) afforded 3-[[(1,1-dimethylethyl)dimethylsilyl]oxy]benzonitrile (9 g, 92%) as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07217728B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-808a371d0be04f619c2727f0df2e1c1c |
| Source note | uspto-grants-2007_05 |