HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonium Hydroxide → 4,6-Bis(1,1-dimethylethyl)-5-hydroxy 2-methylpyrimidine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonium Hydroxide | HCID 14923 | — |
| Edukt | 1-[4-(1,1-Dimethylethyl)-2-methyl-5-oxazolyl]-2,2-dimethyl-1-propanone | HCID 18925378 | — |
| Produkt | 4,6-Bis(1,1-dimethylethyl)-5-hydroxy 2-methylpyrimidine | HCID 9877866 | 75% |
Reaktionsschritte
A mixture of 1-[4-(1,1-dimethylethyl)-2-methyl-5-oxazolyl]-2,2-dimethyl-l-propanone (8.5 g, and concentrated ammonium hydroxide (100 mi) is heated at 180° C. for 36 hours in a steel bomb. The reaction mixture is cooled and the excess ammonia is evaporated on the rotovap. The pH of the resulting mixture is adjusted to pH 6 with concentrated HCl with ice bath cooling. The product is extracted into ether (3×250 mL) and the organic layer is dried (MgSO4) and evaporated. The residue is purified by flash chromatography (silica, 7% EtOAc/hexane) to give pure 4,6-bis(1,1-dimethylethyl)-5-hydroxy-2-methylpyrimidine (6.35g, 75%) as a partial hydrate; mp 62°-65° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05302597 |
| Quelldatensatz | uspto-grants-1994_04 |
| ORD ID | ord-1215a694976146d98ae24f8325fef266 |
| Quellennotiz | uspto-grants-1994_04 |