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

HRID 635904

반응식

HRID 635904 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-189a043104d84f949f287bc8269b7434
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06191164B1

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