HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dichloroacetyl chloride → Benoxacor
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dichloroacetyl chloride | HCID 6593 | — |
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | 3-Methyl-3,4-dihydro-2H-1,4-benzoxazine | HCID 2763760 | — |
| Lösungsmittel | Benzene | HCID 241 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | Benoxacor | HCID 62306 | 83% |
Reaktionsschritte
5.3 ml (55 mmoles) of dichloroacetyl chloride are added dropwise, at a temperature of 20° to 25° C. and while stirring, to a suspension of 7.5 g (50 mmoles) of 2,3-dihydro-3-methyl-1,4-benzoxazine and 5.8 g (55 mmoles) of sodium carbonate in 120 ml of benzene. The reaction mixture is then stirred at the same temperature for 30 minutes and is then taken up in a mixture of water and ethyl acetate. The organic phase is washed with saturated sodium chloride solution, dried over sodium sulfate and evaporated. Crystallising the residue from diisopropyl ether gives 10.8 g of 4-dichloroacetyl-2,3-dihydro-3-methyl-1,4-benzoxazine, melting point 105°-107° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04601745 |
| Quelldatensatz | uspto-grants-1986_07 |
| ORD ID | ord-575aa25dc6ff485985743d86433e5a8e |
| Quellennotiz | uspto-grants-1986_07 |