Реакция #65471

ord-2baf2abaa2e844ce974413592e8f617b

Растворители

Условия реакции

Температура
96°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеequipped with a reflux condenser
  2. 2
    ДругоеThe solvent is evaporated under reduced pressure
  3. 3
    Другоеthe organic phase is separated
  4. 4
    Промывкаwashed with water
  5. 5
    Сушкаdried over sodium sulphate
  6. 6
    Другоеthe solvent is evaporated under reduced pressure

Методика

9.0 g (0. 0444 mol) of 1-(2-cyclopropylphenyl)piperazine, 200 ml of dimethylformamide, 17.5 g (0.0444 mol) of 3-bromo-N-methyl-N-(triphenylmethyl)propanamine and 9 g of potassium carbonate are introduced into a 500 ml round-bottomed flask equipped with a reflux condenser and placed under nitrogen, and the mixture is heated three times for 6 h at 96° C. The solvent is evaporated under reduced pressure, the residue is taken up with water and dichloromethane, the organic phase is separated, washed with water, dried over sodium sulphate and the solvent is evaporated under reduced pressure. There are obtained 4.17 g of 3-[4-(2-cyclopropylphenyl)piperazin-1-yl]-N-methyl-N-(tri-phenylmethyl)propanamine in the form of an oil which is dissolved in 200 ml of methanol, a stream of gaseous hydrochloric acid is passed therein for 10 min, the mixture is concentrated, allowed to stand for 2 days and the precipitate is separated by filtration. 2.94 g of compound are obtained.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05420130uspto-grants-1995_05