HRID2052068

反应详情

EQUATION

反应方程式

HRID 2052068 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1.5 g (0.004 mole) of methyl N-(1-methylimidazol-2-yl)-N'-phenylcarbamimidothioate hydroiodide and 0.73 g (0.0084 mole) of morpholine in 30 ml of t-BuOH is refluxed overnight. Upon cooling, ether is added and morpholine hydroiodide is removed by filtration. The filtrate is taken to dryness and the residue is taken up in CH2Cl2 and converted to the free base with 3 N NaOH. The organic layer is separated, dried over K2CO3, filtered and the solvent is removed in vacuo to give a residue of N-(1-methylimidazol-2-yl)-N'-phenyl-4-morpholine carboximidamide, which is taken up in acetone and converted to the hydrochloride salt with ethereal HCl.

WORKUP

后处理

  1. temperatureUpon cooling
  2. custommorpholine hydroiodide is removed by filtration
  3. customThe organic layer is separated
  4. dry with materialdried over K2CO3
  5. filtrationfiltered
  6. customthe solvent is removed in vacuo