HRID2290899

反应详情

EQUATION

反应方程式

HRID 2290899 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

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.

WORKUP

后处理

  1. customan additional 30 minutes
  2. customat room temperature
  3. extractionthe product was extracted with ether
  4. dry with materialthe extract was dried (magnesium sulfate)
  5. concentrationconcentrated in vacuo
  6. customFinal purification
  7. customthe solvent was removed in vacuo