Реакция #3940

ord-0956ad0caa5041f28456e5e148238e1e

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеan additional 30 minutes
  2. 2
    Другоеat room temperature
  3. 3
    Экстракцияthe product was extracted with ether
  4. 4
    Сушкаthe extract was dried (magnesium sulfate)
  5. 5
    Концентрированиеconcentrated in vacuo
  6. 6
    ДругоеFinal purification
  7. 7
    Другоеthe solvent was removed in vacuo

Методика

15.7 g of 1-bromo-3-chloropropane were added to a cooled solution of 15.0 g of 1-(4-chlorobenzyl)homopiperazine and 12.0 g of potassium hydroxide in 50 ml of dimethyl sulfoxide. The mixture was stirred at 5°-10° C. for one hour, and then an additional 30 minutes at room temperature. After the addition of ice water, the product was extracted with ether, and the extract was dried (magnesium sulfate) and concentrated in vacuo. Final purification was effected on a silica gel column (methylene chloride:methanol, 9:1), and the solvent was removed in vacuo to give 8.4 g (42% of theory) of 1-(4-chlorobenzyl)-4-(3-chloropropyl)homopiperazine as an oil.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04722926uspto-grants-1988_02