HRID258823

反应详情

EQUATION

反应方程式

HRID 258823 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 8 parts of 4-{[4-(diphenylmethyl)-1-piperidinyl]methyl}benzenamine in 50 parts of acetic acid is added 5 parts of acetic anhydride. The resultant mixture is heated to the boiling point under reflux and maintained thereat for 10 minutes, then stripped of solvents by vacuum distillation. The residue is combined with 10 volumes of water. The resultant mixture is made alkaline with concentrated ammonium hydroxide. The mixture thus obtained is extracted with dichloromethane. The dichloromethane extract is dried over anhydrous potassium carbonate and then stripped of solvent by vacuum distillation. The residue, recrystallized from benzene, affords N-acetyl-4-{[4-(diphenylmethyl)-1-piperidinyl]methyl}benzenamine melting at approximately 182°-183°. The product has the formula ##STR5##

WORKUP

后处理

  1. temperatureunder reflux
  2. temperaturemaintained
  3. distillationstripped of solvents by vacuum distillation
  4. customThe mixture thus obtained
  5. extractionis extracted with dichloromethane
  6. extractionThe dichloromethane extract
  7. dry with materialis dried over anhydrous potassium carbonate
  8. distillationstripped of solvent by vacuum distillation
  9. customThe residue, recrystallized from benzene