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

HRID 1916627

反応式

HRID 1916627 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 589705326-Bromo-2-(bromomethyl)quinoline

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-eeef34e06cb945688a8dc1fc86e388de
出典データセット
uspto-grants-2013_12
特許番号
US08618132B2

関連ノート

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