HRID542441

反应详情

EQUATION

反应方程式

HRID 542441 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of 50 g of 3-amino quinuclidine and 40 ml of benzaldehyde in 1000 ml of toluene is brought to reflux for 45 minutes, while eliminating the water formed. Then the solvent is evaporated, the residue is dissolved in 800 ml of methanol and 15 g of potassium borohydride are added within 3 hours while maintaining the temperature at 0° C. Then the solvent is evaporated, the residue is taken up in water, the mixture obtained is extracted with ethyl acetate (or with chloroform), dried on sodium (or magnesium) sulfate, filtered and the filtrate is evaporated. Thus 85 g (yield ≃100%) of the pure expected product are obtained (one spot in TLC) which is in liquid form.

WORKUP

后处理

  1. temperatureto reflux for 45 minutes
  2. customformed
  3. customThen the solvent is evaporated
  4. dissolutionthe residue is dissolved in 800 ml of methanol
  5. addition15 g of potassium borohydride are added within 3 hours
  6. customThen the solvent is evaporated
  7. customthe mixture obtained
  8. extractionis extracted with ethyl acetate (or with chloroform)
  9. dry with materialdried on sodium (or magnesium) sulfate
  10. filtrationfiltered
  11. customthe filtrate is evaporated