HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sulfuric Acid → N,N-dimethyl-N-[2-(7-hydroxy-1H-indazol-4-yl)ethyl]amine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sulfuric Acid | HCID 1118 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | N,N-dimethyl-N-[2-(7-amino-1H-indazol-4-yl)ethyl]amine | HCID 13629325 | — |
| Produkt | N,N-dimethyl-N-[2-(7-hydroxy-1H-indazol-4-yl)ethyl]amine | HCID 13629326 | — |
Reaktionsschritte
In an autoclave, 1.2 g of N,N-dimethyl-N-[2-(7-amino-1H-indazol-4-yl)ethyl]amine and 24 ml of 1N sulfuric acid are heated under argon for 16 hours to 180° C. Subsequently the mixture is combined under ice cooling with sodium bicarbonate and extracted by shaking with ethyl acetate/butanol (10:1). The organic phase is dried, concentrated, and the residue is triturated with ethyl acetate, thus obtaining 700 mg of N,N-dimethyl-N-[2-(7-hydroxy-1H-indazol-4-yl)ethyl]amine, mp 233°-234° C., yielding after treatment with methanol and ethereal hydrochloric acid, and recrystallization from methanol/diethyl ether, 680 mg of N,N-dimethyl-N-[2-(7-hydroxy-1H-indazol-4-yl)ethyl]amine, hydrochloride, mp 223°-227° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04958026 |
| Quelldatensatz | uspto-grants-1990_09 |
| ORD ID | ord-32cbd6824bc2499ba13a8bed93d8e428 |
| Quellennotiz | uspto-grants-1990_09 |