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

HRID 635904

反応式

HRID 635904 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-189a043104d84f949f287bc8269b7434
出典データセット
uspto-grants-2001_02
特許番号
US06191164B1

関連ノート

読み込み中…