Azobisisobutyronitrile → 4-bromo-6-cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran

HRID 635904

Reaktionsgleichung

Reaktionsgleichung von HRID 635904
[Br:1]N1C(=O)CCC1=O.N(C(C)(C)C#N)=NC(C)(C)C#N.[C:21]([C:23]1[CH:24]=[C:25]2[C:30](=[CH:31][CH:32]=1)[O:29][C:28]([CH3:34])([CH3:33])[CH2:27][CH2:26]2)#[N:22]>C(Cl)(Cl)(Cl)Cl>[Br:1][CH:26]1[C:25]2[C:30](=[CH:31][CH:32]=[C:23]([C:21]#[N:22])[CH:24]=2)[O:29][C:28]([CH3:34])([CH3:33])[CH2:27]1

Komponenten

5

Edukt 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 109212656-Cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran

Produkt 1

HCID 102446284-bromo-6-cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 5943Carbon TetrachlorideLösungsmittel

Versuchsvorschrift

11 mmol of N-bromosuccinimide and 0.22 g of azobisisobutyronitrile (Aldrich) are added to a solution of 10 mmol of 6-cyano-2,2-dimethyl-chroman in 30 ml of carbon tetrachloride and the suspension thus obtained is heated to boiling under a reflux condenser for 3 hours. Insoluble succinimide is then filtered off, the solvent is distilled off and the residue is crystallized under a mixture of n-hexane and diisopropyl ether.

Aufarbeitung

  1. customthe suspension thus obtained
  2. temperatureis heated
  3. filtrationInsoluble succinimide is then filtered off
  4. distillationthe solvent is distilled off
  5. customthe residue is crystallized under a mixture of n-hexane and diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-189a043104d84f949f287bc8269b7434
Quelldatensatz
uspto-grants-2001_02
Patentnummer
US06191164B1

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