HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Phosphorus oxychloride → 4,7-Dichloro-6-nitroquinazoline
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Phosphorus oxychloride | HCID 24813 | — |
| Edukt | Phosphorus pentachloride | HCID 24819 | — |
| Edukt | 7-Chloro-6-nitroquinazolin-4(1H)-one | HCID 135687504 | — |
| Produkt | 4,7-Dichloro-6-nitroquinazoline | HCID 10490455 | — |
Reaktionsschritte
7-Chloro-6-nitro-quinazolin-4-one (1.002 g, 4.44mmol), phosphorous oxychloride (11.5 g, 7.51 mmol) and phosphorous pentachloride (1.62 g, 7.74 mmol) were refluxed for 2 hours and the reaction mixture was concentrated in vacuo to a residue which was triturated with toluene and then again with chloroform and dried in vacuo to afford crude 4,7-dichloro-6-nitro-quinazoline. This was dissolved in 35 mL of isopropyl alcohol and 3-ethynylaniline (639 mg, 5.45 mmol) and refluxed for 3 hours. The cooled reaction mixture was filtered to afford the title product as a solid which was washed with 10 mL of isopropyl alcohol and dried in vacuo at 70° C., 1.055 g (66%); mp 230.8°-232.6° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05747498 |
| Quelldatensatz | uspto-grants-1998_05 |
| ORD ID | ord-9851bd02d0fe4cd7b1691377c358dc88 |
| Quellennotiz | uspto-grants-1998_05 |