HRID1313

反应详情

EQUATION

反应方程式

HRID 1313 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

36.8 g (0.138 mol) of 1-benzyl-3-benzylaminopyrrolidine are hydrogenated in 160 ml of methanol over 5 g of 5% strength palladium on active charcoal at 130° C. under a hydrogen pressure of 100 bar for 10 hours. The catalyst is filtered off and 16.6 g (0.138 mol ) of 71% strength pivalaldehyde are added to the filtrate, while stirring, after which the temperature rises from 20° C. to 28° C. The mixture is subsequently stirred for 30 minutes, the methanol is removed on a rotary evaporator and the residue is distilled. 12.7 g of 3-(2,2-dimethyl-propylidene-amino)-pyrrolidine of boiling point: 61° C./10 mbar are obtained with a purity, determined by gas chromatography, of 97%, corresponding to a yield of 58% of theory.

WORKUP

后处理

  1. customfor 10 hours
  2. filtrationThe catalyst is filtered off
  3. addition16.6 g (0.138 mol ) of 71% strength pivalaldehyde are added to the filtrate
  4. customrises from 20° C. to 28° C
  5. stirringThe mixture is subsequently stirred for 30 minutes
  6. customthe methanol is removed on a rotary evaporator
  7. distillationthe residue is distilled