HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonia → Methyl 2-(3,4-dichlorobenzyl)-4-oxo-3,4-dihydroquinazoline-7-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonia | HCID 222 | — |
| Edukt | (3,4-Dichlorophenyl)acetonitrile | HCID 76690 | — |
| Edukt | Dimethyl aminoterephthalate | HCID 79336 | — |
| Lösungsmittel | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| Produkt | Methyl 2-(3,4-dichlorobenzyl)-4-oxo-3,4-dihydroquinazoline-7-carboxylate | HCID 136330126 | — |
Reaktionsschritte
420 Milligrams of dimethyl aminoterephthalate and 446 mg of 3,4-dichlorophenylacetonitrile were added to 10 mL of 4N hydrogen chloride dioxane solution and stirred for about 2 days. Pouring the reaction mixture into ice, its pH was adjusted to 8-9 with 25% aqueous ammonia. The precipitated crystals were recovered by filtration and washed with water. The crude crystals were dissolved in chloroform-ethyl acetate (1:1) mixed solvent, and after removing the insoluble matter by filtration, the remaining solution was concentrated. The residue was purified on silica gel column chromatography (hexane:ethyl acetate=4:1) to provide 253 mg of the title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08101624B2 |
| Quelldatensatz | uspto-grants-2012_01 |
| ORD ID | ord-5444c3375e774297a36f0e4c0ad68e6b |
| Quellennotiz | uspto-grants-2012_01 |