Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 4,6-Dichloro-2,5-dimethylpyrimidine | HCID 237013 | — |
| Edukt | 2,4,6-Trimethylphenylacetonitrile | HCID 520698 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | HCID 21912078 | HCID 21912078 | 106,3% |
Reaktionsschritte
To a solution of mesitylacetonitrile (0.900 g, 5.65 mmol) in 8 ml dry THF was added sodium hydride (60% in oil, 0.250 g, 6.21 mmol) and the mixture was stirred at room temperature for 40 minutes. 2,5-Dimethyl-4,6-dichloropyrimidine (1.000 g, 5.65 mmol) was added and the resulting mixture was heated at reflux for 5 hours. The mixture was quenched with water and extracted with ethyl acetate. The organic layer was dried and concentrated to give 1.800 g of a yellow oil. The oil residue was purified through silica gel column chromatography using 10% ethyl acetate in hexane as eluent to give 0.986 g (58.3%) of the title compound as a white solid, mp 100-102° C. 1H NMR (CDCl3) δ 6.86 (s, 2H), 5.60 (s, 1H), 2.69 (s, 3H), 2.25 (s, 3H), 2.18 (s, 6H), 1.92 (s, 3H) ppm.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US06956047B1 |
|---|
| Quelldatensatz | uspto-grants-2005_10 |
|---|
| ORD ID | ord-3e8f66468e9d436d8ca19eb479cc6b02 |
|---|
| Quellennotiz | uspto-grants-2005_10 |
|---|