HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dimethoxyethane → HCID 66924340, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dimethoxyethane | HCID 8071 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 2-Fluoro-6-iodobenzonitrile | HCID 522722 | — |
| Reactant | (3-Chlorophenyl)boronic acid | HCID 2734323 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 66924340 | HCID 66924340 | 32.1% |
Reaction Steps
In a dry round bottom flask were added 2-fluoro-6-iodobenzonitrile (500 mg; 2.02 mmol), 3-chlorophenyl boronic acid (380 mg; 2.43 mmol), sodium carbonate (2.32 g; 21.86 mmol), tetrakis(triphenylphosphine)palladium(0) (77 mg; 0.07 mmol), DME (20 mL) and water (20 mL) and heated to reflux for 8 hours. The reaction mixture was cooled to room temperature and extracted with ethyl acetate (3×), washed with brine (1×) and water (1×). Organic layers were combined and dried over sodium sulfate and then filtered and solvent removed to yield crude material which was purified by column chromatography (4% ethyl acetate/hexane) to obtain 150 milligrams of 3′-chloro-3-fluorobiphenyl-2-carbonitrile.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07888366B2 |
| Source dataset | uspto-grants-2011_02 |
| ORD ID | ord-fba3d73d9ce549a49938e78c20b8fa1d |
| Source note | uspto-grants-2011_02 |