HRID542442

反应详情

EQUATION

反应方程式

HRID 542442 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

To a solution of 73.7 g of 3-benzylamino quinuclidine in water (≃300 to 400 ml) are added, while cooling to 5° C., 51 ml of a 40% aqueous formaldehyde solution. Then after the addition, the mixture is left for 30 minutes at 5° C., then 32 g of sodium cyanoborohydride are added within 1 to 2 hours. Then it is left at room temperature for 12 hours, extracted with ethyl acetate, the mixture obtained is dried on sodium (or magnesium) sulfate, filtered, the filtrate is evaporated and the residue is distilled (Boiling point [0.04 mm/Hg]=125° C.). Thus the expected product is obtained practically quantitatively.

WORKUP

后处理

  1. additionThen after the addition
  2. waitThen it is left at room temperature for 12 hours
  3. extractionextracted with ethyl acetate
  4. customthe mixture obtained
  5. dry with materialis dried on sodium (or magnesium) sulfate
  6. filtrationfiltered
  7. customthe filtrate is evaporated
  8. distillationthe residue is distilled (Boiling point [0.04 mm/Hg]=125° C.)