HRID2309030

反应详情

EQUATION

反应方程式

HRID 2309030 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The procedure described in Example 12 is followed using 1[3-(4-chlorophenyl)propyl]-piperazine (4.8 g), bis(2-chloroethyl) disulfide (1.9 g), potassium hydroxide (5.0 g), and dimethylsulfoxide (50 ml). Workup as described in Example 12 provides an oil which is purified on a silica gel column (methylene chloride:methanol, 9:1). The resulting oil (1.5 g) is precipitated with ethereal hydrochloric acid and recrystallized from water/ethanol to give 1,1'-(dithiodi-2, 1-ethanediyl)bis{4-[3-(4-chlorophenyl)propyl]piperazine} tetrahydrochloride as a white crystalline solid, m.p. 284°-286° C.

WORKUP

后处理

  1. customprovides an oil which
  2. customis purified on a silica gel column (methylene chloride:methanol, 9:1)
  3. customThe resulting oil (1.5 g) is precipitated with ethereal hydrochloric acid
  4. customrecrystallized from water/ethanol