HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → 4-(4-Fluorophenyl)benzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Benzonitrile, 4-bromo- | HCID 12162 | — |
| Reactant | 4-Fluorophenylboronic acid | HCID 285645 | — |
| Reactant | Potassium Fluoride | HCID 522689 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Solvent | Water | HCID 962 | — |
| Product | 4-(4-Fluorophenyl)benzonitrile | HCID 1393040 | 96.8% |
Reaction Steps
To a solution of 4-bromobenzonitrile (4.0 g, 22 mmol) and 4-fluorophenylboronic acid (4.6 g, 32 mmol) in 4:1 toluene:water (100 mL) were added potassium fluoride (3.8 g, 66 mmol) and Pd(PPh3)4 (2.5 g, 2.2 mmol). The resulting mixture was stirred at reflux for 12 h. The mixture was cooled to room temperature and extracted with ethyl acetate (30 mL*3). The combined organic layers were washed with water, brine, dried over anhydrous Na2SO4 and concentrated under reduced pressure. Purification of the crude residue by silica gel chromatography gave 4′-fluorobiphenyl-4-carbonitrile (4.2 g) as a colorless solid. 1H NMR (400 MHz, CD3OD) δ 7.69 (s, 4H), 7.63-7.60 (m, 2H), 7.15-7.10 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08809342B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-4cc8e04a1b8b4c8c9d54b8aeac977133 |
| Source note | uspto-grants-2014_08 |