HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine hydrochloride → HCID 178443719, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine hydrochloride | HCID 11130 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Sodium Azide | HCID 33557 | — |
| Edukt | 2-Hydroxyoctyloxy-benzonitrile | HCID 68586479 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | HCID 178443719 | HCID 178443719 | — |
Reaktionsschritte
A slurry of 2-hydroxyoctyloxy-benzonitrile (247 mg; 1 mmol), sodium azide (195 mg; 3 mmol), triethylamine hydrochloride (411 mg; 3 mmol) was refluxed in toluene (5 mL) under N2 for 4 hours after which time the reaction mixture was poured onto H2O 0 (10 mL). The precipitate formed was dissolved by addition of 10 M NaOH (aq) and EtOAc. The organic phase was isolated and extracted with 4 M NaOH (aq). The combined aqueous phases was acidified using 12 M HCl (aq) and the precipitate formed isolated by filtration to yield 240 mg (82%) as a purple solid after drying. Mp. 142-146° C. MS (Direct; Cl): 291 (MH+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07741352B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-70b8d520b1d24c98a4f70045adf5d441 |
| Quellennotiz | uspto-grants-2010_06 |