HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → 3-Ethenyl-2,6-difluorobenzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | 3-Cyano-2,4-difluorophenyl trifluoromethanesulfonate | HCID 86727059 | — |
| Catalyst | HCID 178418807 | HCID 178418807 | — |
| Product | 3-Ethenyl-2,6-difluorobenzonitrile | HCID 86727060 | — |
Reaction Steps
3-Cyano-2,4-difluorophenyl trifluoromethanesulfonate (5.20 g, 18.1 mmol), potassium vinyl trifluoroborate (4.85 g, 36.2 mmol), PdCl2(dppf)-CH2Cl2 Adduct (0.662 g, 0.905 mmol), and TEA (5.05 mL, 36.2 mmol) were added to 75 mL of ethanol. The reaction mixture was degassed then heated at reflux for 4 h. LC-MS analysis confirmed product peak. The reaction mixture was diluted with ethyl acetate, washed twice with brine, dried, and evaporated to dryness. The crude material was then purified by MPLC chromatography through a 330 g Redi-sep column eluting with 10% EtOAc/Hexane solvent system to yield 3-ethenyl-2,6-difluorobenzonitrile.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09206199B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-ea8dbff2fa5d4f8b89cf845585d25a44 |
| Source note | uspto-grants-2015_12 |