HRID1277417

反应详情

EQUATION

反应方程式

HRID 1277417 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 6.9 gm (0.03 mol) of clonidine, 5.6 gm of 4-bromo-2-methyl-1-butene, and 5 ml of triethylamine in 25 ml of toluene was heated for 24 hours at 120° C. After cooling, the solvent was decanted, and the residue remaining was dissolved in 1 N hydrochloric acid. After extraction with ether several times (the ethereal extracts were abandoned), the solution was extracted with ether in fractions at stepwisely rising pH values (alkalizing with 2 N sodium hydroxide solution). The thin-layer chromatographically uniform ether extracts were united and dried over MgSO4, and the ether was evaporated in vacuo.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe solvent was decanted
  3. dissolutionthe residue remaining was dissolved in 1 N hydrochloric acid
  4. extractionAfter extraction with ether several times (the ethereal extracts
  5. extractionwas extracted with ether in fractions
  6. dry with materialdried over MgSO4
  7. customthe ether was evaporated in vacuo