反应 #3940

ord-0956ad0caa5041f28456e5e148238e1e

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他an additional 30 minutes
  2. 2
    其他at room temperature
  3. 3
    萃取the product was extracted with ether
  4. 4
    干燥the extract was dried (magnesium sulfate)
  5. 5
    浓缩concentrated in vacuo
  6. 6
    其他Final purification
  7. 7
    其他the solvent was removed in vacuo

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04722926uspto-grants-1988_02