HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium fluoride → 4-(p-Chlorophenyl)-3-fluoro-4-methyl-2-pentenenitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium fluoride | HCID 25953 | — |
| Reactant | Ethyl acetate hexane | HCID 21226206 | — |
| Reactant | 4-(p-Chlorophenyl)-4-methyl-2-pentynenitrile | HCID 21995534 | — |
| Reactant | Potassium fluoride, 99%, spray-dried | HCID 53443437 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-(p-Chlorophenyl)-3-fluoro-4-methyl-2-pentenenitrile | HCID 54269028 | 76.8% |
Reaction Steps
A mixture of cesium fluoride (41.38 g, 0.272 mol), potassium hydrogen fluoride (10.64 g, 0.136 mol) and water (13.07 g, 0.726 mol) in N,N-dimethylformamide is stirred for 10 minutes, treated with a solution of 4-(p-chlorophenyl)-4-methyl-2-pentynenitrile (18.5 g, 0.091 mol) in N,N-dimethylformamide, stirred at 80-85° C. for 4 hours, stirred at room temperature overnight and diluted with water. The aqueous mixture is extracted with ethyl acetate. The organic extracts are combined, washed with water, dried over anhydrous sodium sulfate and concentrated in vacuo to obtain a residue. Column chromatography of the residue using silica gel and a 1:9 ethyl acetate/hexane solution gives the title product as an oil (15.6 g, 76.8% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06235754B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-70d2c4993ec342b99830239e217e7f0e |
| Source note | uspto-grants-2001_05 |