HRID126861

反应详情

EQUATION

反应方程式

HRID 126861 的结构方程式

PROCEDURE

实验过程

A mixture of 58 parts of ethyl α-cyano-1-(phenylmethyl)-4-piperidineacetate and 125 parts of sodium hydroxide solution 2 N is stirred for 3 hours at room temperature. The mixture is neutralized with concentrated hydrochloric acid while cooling and the solvent is evaporated. The residue is stirred for 4 hours at 150° C. in 180 parts of N,N-dimethylacetamide. The reaction mixture is cooled, filtered and the filtrate is evaporated. The residue is taken up in water and extracted with methylbenzene. The extract is dried, filtered and evaporated. The residue is distilled, yielding 35 parts (82%) of 1-(phenylmethyl)-4-piperidineacetonitrile; bp. 135°-140° C. at 0.2-0.3 mm. pressure.

WORKUP

后处理

  1. temperaturewhile cooling
  2. customthe solvent is evaporated
  3. stirringThe residue is stirred for 4 hours at 150° C. in 180 parts of N,N-dimethylacetamide
  4. temperatureThe reaction mixture is cooled
  5. filtrationfiltered
  6. customthe filtrate is evaporated
  7. extractionextracted with methylbenzene
  8. customThe extract is dried
  9. filtrationfiltered
  10. customevaporated
  11. distillationThe residue is distilled