HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydroxylamine → 8-Bromo-(1,2,4)triazolo(1,5-a)pyridin-2-amine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydroxylamine | HCID 787 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | Ethyl aminon-(3-bromopyridin-2-YL)methanethiocarbamate | HCID 59199107 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 8-Bromo-(1,2,4)triazolo(1,5-a)pyridin-2-amine | HCID 46864069 | — |
Reaktionsschritte
Hydroxylamine (58.5 g, 842 mmol) and N,N-diisopropylethylamine (65.3 g, 86.3 mL, 505 mmol) were dissolved in methanol (200 mL) and ethanol (200 mL). N-(3-Bromo-pyridin-2-yl)-N′-ethoxycarbonyl-thiourea (51.2 g, 168 mmol) was added and the reaction mixture was stirred at room temperature for 1 hour and then at 60° C. for 3 hours. The white precipitate was filtered off and triturated with water for 25 minutes, filtered and triturated two times with diethylether. The solid was dried by co-evaporation with toluene and dried in vacuum. The title compound was obtained as a white solid (27.9 g, 78%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08486967B2 |
| Quelldatensatz | uspto-grants-2013_07 |
| ORD ID | ord-9dd53110377944a686ae91764f37b753 |
| Quellennotiz | uspto-grants-2013_07 |