HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dimethoxyethane → 4-Methyl-2-phenylpyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dimethoxyethane | HCID 8071 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Phenylboronic Acid | HCID 66827 | — |
| Reactant | 2-Chloro-4-methylpyridine | HCID 77248 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Solvent | Water | HCID 962 | — |
| Product | 4-Methyl-2-phenylpyridine | HCID 77026 | 84.4% |
Reaction Steps
A 1 L round bottom flask was charged with 2-chloro-4-methylpyridine (25 g, 196 mmol), phenylboronic acid (23.9 g, 196 mmol), potassium carbonate (81 g, 588 mmol), Pd(PPh3)4 (2.3 g, 1.9 mmol), dimethoxyethane (500 mL) and water (150 mL). The reaction mixture was degassed with nitrogen and heated to reflux for 22 h. After cooling, the aqueous layer was extracted with EtOAc; the organic portion was combined and subjected to column chromatography (SiO2, 5% EtOAc in hexane to 10% EtOAc in hexane) to give 28 g (78%) of 4-methyl-2-phenylpyridine. The product was confirmed by NMR and GC/MS.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08709615B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-19f5a35878ef4ad98b05452dccc4dd74 |
| Source note | uspto-grants-2014_04 |