HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methyl iodide → 6-Bromo-4-methyl-1,4-benzoxazin-3-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methyl iodide | HCID 6328 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 6-Bromo-2H-1,4-benzoxazin-3(4H)-one | HCID 16218142 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 6-Bromo-4-methyl-1,4-benzoxazin-3-one | HCID 53217383 | — |
Reaktionsschritte
To sodium hydride (63 mg) in DMF (3 mL) under an atmosphere of nitrogen was added 6-bromo-2H-benzo[b][1,4]oxazin-3(4H)-one (0.3 g) and the mixture was stirred at room temperature for 1 h. Methyl iodide (0.123 mL) was added and the mixture was stirred overnight at room temperature. The mixture was poured onto ice/water and extracted into ethyl acetate (×2). The ethyl acetate was washed with water (×3), dried and the solvent was evaporated. The resulting material was purified by chromatography on silica eluting with 10% ethyl acetate/isohexane to afford the sub-titled compound (299 mg).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08193239B2 |
| Quelldatensatz | uspto-grants-2012_06 |
| ORD ID | ord-15e1c4e7f27d4b5d82625a4267c0c832 |
| Quellennotiz | uspto-grants-2012_06 |