HRID2309028

反应详情

EQUATION

反应方程式

HRID 2309028 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-[4-(4-chlorobenzyl)homopiperazin-1-yl]-propanethiol (4.0 g) and 2N sodium hydroxide (50 ml) is stirred at room temperature for 8 days. The product is extracted with ether, dried, and concentrated to give a yellow oil, which is purified on a silica gel column (methylene chloride:methanol, 95:5). The resulting yellow oil (1.5 g) is dissolved in ether and the salt precipitated with ethereal hydrochloric acid. Recrystallization from ethanol provided 1,1'-(dithiodi-3,1-propanediyl)bis[4-(4-chlorobenzyl) homopiperizine] tetrahydrochloride as a white crystalline solid, m.p. >170° (dec.).

WORKUP

后处理

  1. extractionThe product is extracted with ether
  2. customdried
  3. concentrationconcentrated
  4. customto give a yellow oil, which
  5. customis purified on a silica gel column (methylene chloride:methanol, 95:5)
  6. dissolutionThe resulting yellow oil (1.5 g) is dissolved in ether
  7. customthe salt precipitated with ethereal hydrochloric acid
  8. customRecrystallization from ethanol