HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → N-[(6-chloropyridin-3-yl)methyl]-2,2-difluoroethanamine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 2,2-Difluoroethanamine | HCID 136274 | — |
| Edukt | 2-Chloro-5-(chloromethyl)pyridine | HCID 155479 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | N-[(6-chloropyridin-3-yl)methyl]-2,2-difluoroethanamine | HCID 44604123 | 53,9% |
Reaktionsschritte
41.57 g (256.6 mmol) of 2-chloro-5-chloromethylpyridine, 20.80 g (256.6 mmol) of 2,2-difluoroethane-1-amine and 35.8 ml (256.6 mmol) of triethylamine in 500 ml of acetonitrile are stirred at 45° C. for 21 hours. The reaction mixture is concentrated under reduced pressure and the residue is then taken up in 1 N aqueous hydrochloric acid and the mixture is washed with ethyl acetate. The aqueous phase is made alkaline using 2.5 N aqueous sodium hydroxide solution and extracted repeatedly with ethyl acetate. Concentration of the organic phase under reduced pressure gives 28.6 g (53% of theory) of N-[(6-chloropyridin-3-yl)methyl]-2,2-difluoroethane-1-amine.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08106211B2 |
| Quelldatensatz | uspto-grants-2012_01 |
| ORD ID | ord-a97b878cf9b84a64acc021d5d53daabd |
| Quellennotiz | uspto-grants-2012_01 |