HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl Acetate → 6-[4-[4-(Diphenylmethoxy)piperidino]butylamino][1,2,4]triazolo[4,3-b]pyridazine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 6-Chloro-[1,2,4]triazolo[4,3-b]pyridazine | HCID 313624 | — |
| Edukt | 1-Piperidinebutanamine, 4-(diphenylmethoxy)- | HCID 11739259 | — |
| Lösungsmittel | 1-Butanol | HCID 263 | — |
| Produkt | 6-[4-[4-(Diphenylmethoxy)piperidino]butylamino][1,2,4]triazolo[4,3-b]pyridazine | HCID 15524151 | 39,4% |
Reaktionsschritte
1.15 g of 4-(diphenylmethoxy)-1-piperidinebutanamine and 578 mg of 6-chloro[1,2,4]triazolo[4,3-b]pyridazine were dissolved in 20 ml of 1-butanol; 1.17 ml of N-ethyldiisopropylamine was added, followed by refluxing under heating for 14 hours. After cooling, ethyl acetate was added; the reaction mixture was washed with aqueous sodium bicarbonate and saturated saline and dried over magnesium sulfate. After concentration under reduced pressure, the residue was subjected to silica gel column chromatography and eluted with ethyl acetate-methanol-triethylamine (50:5:1). The desired fraction was collected and concentrated under reduced pressure; the residue was crystallized from ethyl acetate and dried to yield 611 mg of the title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06610694B1 |
| Quelldatensatz | uspto-grants-2003_08 |
| ORD ID | ord-b5bf99c2ffe947f096ecd639dfe4e842 |
| Quellennotiz | uspto-grants-2003_08 |