HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 4-(4-Methoxyphenylethynyl)-3-cyanopyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-Ethynyl-4-methoxybenzene | HCID 251020 | — |
| Reactant | 4-Chloro-nicotinonitrile | HCID 13411112 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-(4-Methoxyphenylethynyl)-3-cyanopyridine | HCID 22503235 | 95% |
Reaction Steps
4-Chloro-3-cyanopyridine (1.50 g) and 4-methoxyphenylacetylene (1.60 g) were reacted in the presence of dichlorobistriphenylphosphinepalladium (0.14 g), cuprous iodide (75 mg) and triethylamine (10 ml) in N,N-dimethylformamide (25 ml) in nitrogen atmosphere at 100° C. overnight. The reaction mixture was poured into water (100 ml), and the mixture was extracted with ethyl acetate. The resulting organic layer was washed with water and brine, and dried over magnesium sulfate. The solvent was evaporated, and the resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane system), to give 4-(4-methoxyphenylethynyl)-3-cyanopyridine (2.13 g, 95%) as a pale yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06875761B2 |
| Source dataset | uspto-grants-2005_04 |
| ORD ID | ord-b3b802698bf5432c85e3388da5fac389 |
| Source note | uspto-grants-2005_04 |