HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Chloroacetaldehyde → HCID 18001294, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Chloroacetaldehyde | HCID 33 | — |
| Edukt | 2-Amino-4-chloropyrimidine | HCID 223332 | — |
| Edukt | Sodium Methoxide | HCID 10942334 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 18001294 | HCID 18001294 | 67% |
Reaktionsschritte
2-Amino-4-chloropyrimidine (1.00 g, 7.72 mmol) and sodium methoxide (1.25 g, 23.2 mmol) were suspended in methanol (20 ml) and heated under reflux for 2 h then cooled to ambient temperature. Chloroacetaldehyde (2.4 ml of a 45% w/w solution in water, 15.44 mmol) was added and the mixture heated under reflux for 22 h, allowed to cool to ambient temperature then pre-adsorbed directly onto silica. Purification by chromatography on silica gel eluting with dichloromethane (containing 1% conc. ammonia) on a gradient of methanol (1-4%) gave 7-methoxyimidazo[1,2-a]pyrimidine (0.77 g, 67%) as a white crystalline solid: δH (400 MHz, CDCl3) 4.04 (3H, s), 6.41 (1H, d, J 7), 7.31 (1H, d, J 1), 7.50 (1H, d, J 1), 8.17 (1H, d, J 7).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06642229B2 |
| Quelldatensatz | uspto-grants-2003_11 |
| ORD ID | ord-8e1ea295441a4334beabc5a39142bb53 |
| Quellennotiz | uspto-grants-2003_11 |