Azobisisobutyronitrile → HCID 86725430、化合物

HRID 1525920ノート

反応式

HRID 1525920 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[C:4]([F:14])[CH:3]=1.[Br:15]N1C(=O)CCC1=O.N(C(C)(C)C#N)=NC(C)(C)C#N>C(Cl)(Cl)(Cl)Cl>[Br:15][CH:8]([C:5]1[CH:6]=[CH:7][C:2]([Br:1])=[CH:3][C:4]=1[F:14])[C:9]([O:11][CH2:12][CH3:13])=[O:10]

参加物

5

反応物 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 45790370Ethyl (4-bromo-2-fluorophenyl)acetate

生成物 1

HCID 86725430HCID 86725430、化合物収率 96.1%

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

反応条件

温度
90 °C

実験手順

To a stirring solution of ethyl 2-(4-bromo-2-fluorophenyl)acetate (3.92 g, 15.0 mmol) in carbon tetrachloride (50 mL) was slowly added N-bromosuccinimide (2.67 g, 15.0 mmol) and then azobisisobutyronitrile (0.37 g, 2.3 mmol). The reaction mixture was stirred for 9 h at 90° C. and then cooled to room temperature. The residue was purified by flash chromatography (0-100% ethyl acetate/hexanes) to provide the title product (4.9 g, 96% yield). MS(ES)+ m/e 340.9 [M+H]+.

後処理

  1. temperaturecooled to room temperature
  2. customThe residue was purified by flash chromatography (0-100% ethyl acetate/hexanes)

出典と根拠

ORDレコード
ord-6db28024aaea44daa019a47408d72cb8
出典データセット
uspto-grants-2015_07
特許番号
US09084794B2

反応ノート

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