Azobisisobutyronitrile → HCID 86643710, Verbindung
Reaktionsgleichung
[Cl:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[C:4]([C:9]#[N:10])[N:3]=1.[Br:11]N1C(=O)CCC1=O.CC(N=NC(C#N)(C)C)(C#N)C>C(Cl)(Cl)(Cl)Cl>[Br:11][CH2:8][C:7]1[C:2]([Cl:1])=[N:3][C:4]([C:9]#[N:10])=[CH:5][CH:6]=1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
2-Chloro-6-cyano-3-methylpyridine (92.0 mg, 0.603 mmol) obtained in Step 2 was dissolved in carbon tetrachloride (4 mL), and the mixture was stirred for 1 hour under reflux after adding N-bromosuccinimide (118 mg, 0.663 mmol) and α,α-azobisisobutyronitrile (9.90 mg, 0.0603 mmol). The mixture was concentrated under reduced pressure, and the resulting residue was purified by preparative TLC to give 3-bromomethyl-2-chloro-6-cyanopyridine (55.8 mg, 40%).
Aufarbeitung
- temperatureunder reflux
- concentrationThe mixture was concentrated under reduced pressure
- customthe resulting residue was purified by preparative TLC
Quellen und Nachweise
- ORD-Eintrag
- ord-7d34bfc8be8a4ad488a927da221f98d7
- Quelldatensatz
- uspto-grants-2011_08
- Patentnummer
- US07998954B2
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