HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2-(dimethylamino)-4-(trifluoromethyl)-6H-1,3-oxazin-6-one → 3-(6-Fluoro-3-methyl-1,2-benzisoxazol-5-yl)-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2-(dimethylamino)-4-(trifluoromethyl)-6H-1,3-oxazin-6-one | HCID 3723862 | — |
| Edukt | 6-Fluoro-3-methylbenzo[d]isoxazol-5-amine | HCID 18314470 | — |
| Lösungsmittel | Acetic Acid | HCID 176 | — |
| Produkt | 3-(6-Fluoro-3-methyl-1,2-benzisoxazol-5-yl)-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione | HCID 18314502 | 73,3% |
Reaktionsschritte
A mixture of 5-amino-6-fluoro-3-methyl-1,2-benzisoxazole (4.85 g, 0.029 mol) and 2-dimethylamino-4-(trifluoromethyl)-6H-1,3-oxazin-6-one (6.70 g, 0.0320 mol) in acetic acid is refluxed for 90 minutes, cooled to room temperature, and poured into an ice-water mixture. The resultant aqueous mixture is filtered to obtain a solid. The solid is air-dried and dissolved in ethyl acetate. The resultant organic solution is washed with brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to give the title product as a yellow solid (7.00 g, mp 235-237° C.) which is identified by NMR spectral analyses.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06355796B1 |
| Quelldatensatz | uspto-grants-2002_03 |
| ORD ID | ord-4ce46596b9ed4e759054c3cee9135dc7 |
| Quellennotiz | uspto-grants-2002_03 |