Reaktionsgleichung
[Br:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.[CH3:10][CH2:11][OH:12]>>[CH2:11]([O:12][C:6](=[NH:7])[C:5]1[CH:8]=[CH:9][C:2]([Br:1])=[CH:3][CH:4]=1)[CH3:10]Komponenten
3
Reaktionsbedingungen
- Temperatur
- 2.5 °C
Versuchsvorschrift
4-Bromo-benzonitrile (5 g) was suspended in absolute EtOH (100 ml) and cooled to 0-5° C. HCl gas was bubbled through, initially vigorously for several minutes and later slowly for 5 hours. The resulting solution was allowed to stir overnight. Most of solvent was removed and the precipitate was filtered, washed with EtOH twice and dried to afford compound 2BN (4.1 g) as white solid. (Note: large scale synthesis may take longer time to get reaction complete. It is better to monitor the disappearance of starting material to get reaction end point.)
Aufarbeitung
- customHCl gas was bubbled through, initially vigorously for several minutes
- customMost of solvent was removed
- filtrationthe precipitate was filtered
- washwashed with EtOH twice
- customdried
- customto afford compound 2BN (4.1 g) as white solid
- custom(Note: large scale synthesis
- customto get
- customreaction complete
- customto get
- customreaction end point
Quellen und Nachweise
- ORD-Eintrag
- ord-3748fbfe636f4c7e8440745b1f7f7c83
- Quelldatensatz
- uspto-grants-2014_05
- Patentnummer
- US08716483B2
Verknüpfte Notizen
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