反応 #5850

ord-45d6e0e571fe4728804424dcef92127c

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他A 3000 ml three-necked round bottom flask was equipped with magnetic stirring
  2. 2
    温度The stirring mixture was refluxed for seven hours
  3. 3
    その他During the course of the reaction
  4. 4
    その他a yellow precipitate formed in the reaction mixture
  5. 5
    温度chilled in an ice-water bath

実験手順

A 3000 ml three-necked round bottom flask was equipped with magnetic stirring, a heating mantle, a reflux condenser, and a nitrogen atmosphere. The flask was charged with 4-dodecyl-4'-hydroxyazobenzene (60.0 g, 0.164 mol), 1,10-dibromodecane, (66.95 g, 0.223 mol), potassium hydroxide (9.75 g, 0.174 mol), and ethanol (1260 ml). The stirring mixture was refluxed for seven hours. During the course of the reaction, a yellow precipitate formed in the reaction mixture. The reaction mixture then was cooled to room temperature and chilled in an ice-water bath. A crude product was isolated by suction filtration, washed with water, then with hexane. The product was recrystallized from ethyl acetate.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05246747uspto-grants-1993_09