反应 #3940
ord-0956ad0caa5041f28456e5e148238e1e
反应方程式
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他an additional 30 minutes
- 2其他at room temperature
- 3萃取the product was extracted with ether
- 4干燥the extract was dried (magnesium sulfate)
- 5浓缩concentrated in vacuo
- 6其他Final purification
- 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.