HRID256711

反应详情

EQUATION

反应方程式

HRID 256711 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

9.36 g (0.1 mole) of cyclopropylamine hydrochloride and 8.9 g (0.1 mole) of the sodium salt of cyanoguanidine are suspended in 100 ml of n-butanol and 8 ml of water. The mixture is heated under reflux for 2 hours. The suspension is filtered and the filter cake is washed with 100 ml of n-butanol. The filtrate is evaporated under reduced pressure. The residual oil is taken up in 300 ml of acetonitrile. The mixture is heated to reflux, filtered hot and the filter cake is washed with acetonitrile. The filtrate is evaporated off and the oil obtained crystallizes slowly. 7.7 g of N-cyano-N'-cyclopropylguanidine are obtained. Yield: 62%. M.P.: 106° C. (isopropyl alcohol/diethyl ether).

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 2 hours
  3. filtrationThe suspension is filtered
  4. washthe filter cake is washed with 100 ml of n-butanol
  5. customThe filtrate is evaporated under reduced pressure
  6. temperatureThe mixture is heated
  7. temperatureto reflux
  8. filtrationfiltered hot
  9. washthe filter cake is washed with acetonitrile
  10. customThe filtrate is evaporated off
  11. customthe oil obtained
  12. customcrystallizes slowly