HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl Acetate → N,N-dimethyl-N-[2-(7-nitro-1H-indazol-4-yl)ethyl]amine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Sodium cyanoborohydride | HCID 5003444 | — |
| Edukt | N,N-dimethyl-N-[2-(7-nitro-1H-indazol-4-yl)ethenyl]amine | HCID 54098844 | — |
| Lösungsmittel | Acetic Acid | HCID 176 | — |
| Produkt | N,N-dimethyl-N-[2-(7-nitro-1H-indazol-4-yl)ethyl]amine | HCID 13629307 | 84,5% |
Reaktionsschritte
16.2 g of N,N-dimethyl-N-[2-(7-nitro-1H-indazol-4-yl)ethenyl]amine is dissolved in 200 ml of acetic acid and combined under ice cooling in incremental portions with 6.3 g of sodium cyanoborohydride within 30 minutes. After another 30 minutes, the mixture is combined with ice and ethyl acetate, adjusted to 8-9 with concentrated sodium hydroxide solution, and extracted with ethyl acetate. The solution is dried, concentrated, and the residue recrystallized from ethyl acetate/diisopropyl ether, thus obtaining 13.8 g of N,N-dimethyl-N-[2-(7-nitro-1H-indazol-4-yl)ethyl]amine, mp 145°-146° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04958026 |
| Quelldatensatz | uspto-grants-1990_09 |
| ORD ID | ord-42e58cecc7064844bd4c52925edbe81c |
| Quellennotiz | uspto-grants-1990_09 |