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

HRID 342611

反応式

HRID 342611 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 110115352,6-Dichloro-3-nitrobenzyl Bromide

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b7a568ba3d00424294d137ce07854653
出典データセット
uspto-grants-1999_01
特許番号
US05859025

関連ノート

読み込み中…