HRID258821

反应详情

EQUATION

反应方程式

HRID 258821 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 126 parts of 4-(diphenylmethyl)piperidine in 1200 parts of 95% ethanol is added a solution of 69 parts of sodium carbonate in 1500 parts of water. The resultant mixture is heated at the boiling point under reflux with vigorous stirring while a solution of 112 parts of 4-nitrobenzyl chloride in 800 parts of 95% ethanol is rapidly stirred in, and for 4 hours thereafter. Solvent is then removed by vacuum distillation, and the residue is partitioned between dichloromethane and water. The organic layer is separated, dried over anhydrous potassium carbonate, and stripped of solvent by vacuum distillation. The residue, recrystallized from anhydrous ethanol, affords 1-[(4-nitrophenyl)methyl]-4-(diphenylmethyl)piperidine melting at approximately 130°-131°.

WORKUP

后处理

  1. temperatureunder reflux
  2. customSolvent is then removed by vacuum distillation
  3. customthe residue is partitioned between dichloromethane and water
  4. customThe organic layer is separated
  5. dry with materialdried over anhydrous potassium carbonate
  6. distillationstripped of solvent by vacuum distillation
  7. customThe residue, recrystallized from anhydrous ethanol