3-Phenylprop-2-enenitrile → Cinnamimidamide

Temperatur

0 °C

Cinnamonitrile (25.0 g, 194 mmol) was dissolved in EtOH (ethanol) (200 mL). The solution was cooled to 0° C. and HCl gas bubbled through the solution for 30 minutes. The solution was stirred at ambient temperature for 16 h and then concentrated under vacuum. The residue was dissolved in EtOH (100 mL), cooled to 0° C. and a solution of NH3/MeOH (7M, 69 mL, 484 mmol) was added dropwise through an addition funnel. Once added, the solution was allowed to warm to ambient temperature and the resulting NH4Cl was filtered off. The solution was concentrated under vacuum and the resulting white solid was used without further purification (26 g crude).

1. customHCl gas bubbled through the solution for 30 minutes
2. concentrationconcentrated under vacuum
3. dissolutionThe residue was dissolved in EtOH (100 mL)
4. temperaturecooled to 0° C.
5. additionOnce added
6. temperatureto warm to ambient temperature
7. filtrationthe resulting NH4Cl was filtered off
8. concentrationThe solution was concentrated under vacuum
9. customthe resulting white solid was used without further purification (26 g crude)

ORD-Eintrag

ord-32928aa9dc1446bfab1a8ab258d9abbc

Quelldatensatz

uspto-grants-2010_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07709483B2