Azobisisobutyronitrile → 2,6-Dichloro-3-nitrobenzyl Bromide

HRID 342611

Reaktionsgleichung

Reaktionsgleichung von HRID 342611
[Br:1]C1(Br)NC(=O)NC1=O.[Cl:10][C:11]1[C:16]([N+:17]([O-:19])=[O:18])=[CH:15][CH:14]=[C:13]([Cl:20])[C:12]=1[CH3:21].CC(N=NC(C#N)(C)C)(C#N)C.CC(=O)OCC>ClC1C=CC=CC=1>[Cl:10][C:11]1[C:16]([N+:17]([O-:19])=[O:18])=[CH:15][CH:14]=[C:13]([Cl:20])[C:12]=1[CH2:21][Br:1]

Komponenten

6

Edukt 4

HCID 6547AzobisisobutyronitrileHCID 8857Ethyl AcetateHCID 971552,6-Dichloro-3-nitrotolueneHCID 54068228Dibromohydantoin2×

Produkt 1

HCID 110115352,6-Dichloro-3-nitrobenzyl Bromide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7964ChlorobenzeneLösungsmittel

Versuchsvorschrift

A mixture of dibromohydantoin (70 g, 0.24 mol) and AlBN (5 g) was added in portions at 150° C. to 2,6-dichloro-3-nitrotoluene (100 g, 0.48 mol) in chlorobenzene (400 ml). After 1 h, a mixture of dibromohydantoin (35 g, 0.12 mol) and AIBN (2.5 g) was again added. After a further 1.5 h, the mixture was allowed to cool and EA (500 ml) was added. This mixture was washed once each with saturated Na2SO3, Na2CO3 and NaCl solution, dried (MgSO4) and concentrated, the title compound being obtained as an amorphous powder.

Aufarbeitung

  1. additionwas again added
  2. waitAfter a further 1.5 h
  3. temperatureto cool
  4. washThis mixture was washed once each with saturated Na2SO3, Na2CO3 and NaCl solution
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-b7a568ba3d00424294d137ce07854653
Quelldatensatz
uspto-grants-1999_01
Patentnummer
US05859025

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