HRID2083582

反应详情

EQUATION

反应方程式

HRID 2083582 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Reaction of 2.5 parts of diphenyl-3-pyridylmethane in 60 parts by volume of cyclohexane with an equivalent amount of butyl lithium at 10° C under nitrogen is followed by the addition of 2.1 parts of 4-(2-chloroethyl)-4-azatricyclo[4.3.1.13,8 ]undecane [preparable by mixing the hydrochloride thereof (U.S. Pat. No. 3,845,038) with excess aqueous sodium carbonate, extracting the mixture with toluene, and consecutively washing the extract with water, drying it over anhydrous sodium sulfate, filtering out the drying agent, and removing the solvent by vacuum distillation]. Quenching of the reaction with water and isolation by extraction with ether, washing, drying and evaporation of solvent provides 4-[3,3-(diphenyl)-3-(3-pyridyl)propyl[-4-azatricyclo[4.3.1.13,8 ]undecane having the following structural formula ##STR52##

WORKUP

后处理

  1. extraction3,845,038) with excess aqueous sodium carbonate, extracting the mixture with toluene
  2. washconsecutively washing the
  3. extractionextract with water
  4. dry with materialdrying it over anhydrous sodium sulfate
  5. filtrationfiltering out the drying agent
  6. customremoving the solvent
  7. distillationby vacuum distillation]
  8. customQuenching of the reaction with water and isolation by extraction with ether
  9. washwashing
  10. customdrying
  11. customevaporation of solvent