HRID463217

反应详情

EQUATION

反应方程式

HRID 463217 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

An amount of 4.2 gm (0.0133 mol) of 2-amino-5-(4-phenylsulfinylbutoxy)-benzyl alcohol [prepared from 2-nitro-5-(4-phenylsulfinyl-butoxy)-benzyl alcohol by catalytic hydrogenation] is dissolved in 150 ml of chloroform and mixed with 6.9 gm (0.05 mol) of potassium carbonate. Ten milliliters of a 20% solution of phosgene in toluene is slowly added dropwise to this mixture under stirring. After further stirring for two hours, the solution is washed with water and dried with sodium sulfate, and the solvents are distilled off in vacuo. The residue is recrystallized from ethyl acetate/cyclohexane.

WORKUP

后处理

  1. stirringAfter further stirring for two hours
  2. washthe solution is washed with water
  3. dry with materialdried with sodium sulfate
  4. distillationthe solvents are distilled off in vacuo
  5. customThe residue is recrystallized from ethyl acetate/cyclohexane