HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
3-Chlorophenol → 6,7-Dimethoxyquinazoline
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 3-Chlorophenol | HCID 7933 | — |
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 4-Chloro-6,7-dimethoxyquinazoline | HCID 2769364 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 6,7-Dimethoxyquinazoline | HCID 3031661 | — |
Reaktionsschritte
THF (5 ml) and NaH (60% disp in oil, approx. 28 mg) is added to a dry flask maintained under inert atmosphere at room temperature. m-Chlorophenol (0.09 g) is added as a soin. In THF (1 mL) and stirring Is continued until the solution became clear. 4-Chloro-6,7-dimethoxyquinazoline is added all at once (as the solid) and stirring was maintained overnight at RT. The solution is partitioned between CH2CL2 and 5% NaOH. The organic layer is washed with brine, dried (Na2SO4) and concentrated. Flash column chromatography (40% EtOAc/Hex) provided the pure compound. An analytical sample is obtained by recrystallization from EtOAc/Hex to provide 4-m-chlorophenoxy)-6,7-dimethoxyquinazoline (0.05 g, white needles, m.p. 152°-153° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05646153 |
| Quelldatensatz | uspto-grants-1997_07 |
| ORD ID | ord-933dd18018cd41ea86500644dee26b38 |
| Quellennotiz | uspto-grants-1997_07 |