Azobisisobutyronitrile → 6-Bromo-2-(bromomethyl)quinoline

HRID 1916627

반응식

HRID 1916627 반응식
CC(N=NC(C#N)(C)C)(C#N)C.[Br:13]N1C(=O)CCC1=O.[Br:21][C:22]1[CH:23]=[C:24]2[C:29](=[CH:30][CH:31]=1)[N:28]=[C:27]([CH3:32])[CH:26]=[CH:25]2>C(Cl)(Cl)(Cl)Cl>[Br:21][C:22]1[CH:23]=[C:24]2[C:29](=[CH:30][CH:31]=1)[N:28]=[C:27]([CH2:32][Br:13])[CH:26]=[CH:25]2

참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 5228856-Bromo-2-methylquinoline

생성물 1

HCID 589705326-Bromo-2-(bromomethyl)quinoline

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

148 mg (1.00 mmol) α,α-azoisobutyronitrile and 8.01 g (45.0 mmol) N-bromosuccinimide are added successively to a solution of 10.0 g (45.0 mmol) 6-bromo-2-methyl-quinoline in 60 mL carbon tetrachloride. The reaction mixture is refluxed for 8 h. It is filtered and the filtrate is washed twice with water. The organic phase is dried over MgSO4 and the solvent is eliminated i.vac. The purification is carried out by column chromatography on silica gel (PE/EtOAc 4:1).

후처리

  1. temperatureThe reaction mixture is refluxed for 8 h
  2. filtrationIt is filtered
  3. washthe filtrate is washed twice with water
  4. dry with materialThe organic phase is dried over MgSO4
  5. customThe purification

출처 및 근거

ORD 기록
ord-eeef34e06cb945688a8dc1fc86e388de
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08618132B2

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