HRID2309028
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- extractionThe product is extracted with ether
- customdried
- concentrationconcentrated
- customto give a yellow oil, which
- customis purified on a silica gel column (methylene chloride:methanol, 95:5)
- dissolutionThe resulting yellow oil (1.5 g) is dissolved in ether
- customthe salt precipitated with ethereal hydrochloric acid
- customRecrystallization from ethanol