Реакция #5849

ord-1a0b05586da349f5b4252b3b31d4054d

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеA 3000 ml three-necked round bottom flask was equipped with magnetic stirring
  2. 2
    workup.ADDITIONThe flask was charged with 4-dodecyl-4
  3. 3
    ТемператураThe solution was refluxed for seven hours
  4. 4
    ДругоеDuring the course of the reaction
  5. 5
    Другоеa yellow precipitate formed in the reaction mixture
  6. 6
    Температураchilled in an ice-water bath

Методика

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 solution was refluxed for seven hours. During the course of the reaction, a yellow precipitate formed in the reaction mixture. The reaction mixture 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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05246748uspto-grants-1993_09