HRID280848

反应详情

EQUATION

反应方程式

HRID 280848 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Pentylamine (17.43 g, 0.20 mol) in 2-propanol (175 ml) was acidified with conc. HCl (17 ml, 0.204 mol) and then treated with sodium dicyanamide (23.15 g, 0.26 mol). The mixture was refluxed for 20 hours, allowed to cool and filtered through diatomaceous earth. The filtrate was concentrated in vacuo and the residue dissolved in chloroform. This solution was washed with water and dried over magnesium sulfate. Filtration and evaporation in vacuo gave 20.93 g (67.9%) of off-white solid; mass spec.: M+ at 154.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 20 hours
  2. temperatureto cool
  3. filtrationfiltered through diatomaceous earth
  4. concentrationThe filtrate was concentrated in vacuo
  5. dissolutionthe residue dissolved in chloroform
  6. washThis solution was washed with water
  7. dry with materialdried over magnesium sulfate
  8. filtrationFiltration and evaporation in vacuo