HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diethyl Ether → 6-chloro-8-methoxy-1H-benzo[d][1,3]oxazine-2,4-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diethyl Ether | HCID 3283 | — |
| Edukt | Triphosgene | HCID 94429 | — |
| Edukt | 2-Amino-5-chloro-3-methoxybenzoic acid | HCID 54595874 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 6-chloro-8-methoxy-1H-benzo[d][1,3]oxazine-2,4-dione | HCID 86670580 | — |
Reaktionsschritte
To 2-amino-5-chloro-3-methoxybenzoic acid (0.72 g, 3.57 mmol) in anhydrous tetrahydrofuran (15 mL) was added triphosgene (0.53 g, 1.8 mmol). The mixture was heated to refluxed under a nitrogen atmosphere for 2.5 hours. The resulting solution was cooled to ambient temperature, diethyl ether (10 mL) was added, which caused a solid to precipitate. The solid was collected by filtration and washed with more diethyl ether to yield 6-chloro-8-methoxy-1H-benzo[d][1,3]oxazine-2,4-dione. MS (m/z): 226.3, 228.3 (M+H)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08673897B2 |
| Quelldatensatz | uspto-grants-2014_03 |
| ORD ID | ord-77b0c302418546b1a5642a4a9d4b7251 |
| Quellennotiz | uspto-grants-2014_03 |