HRID1577804

反应详情

EQUATION

反应方程式

HRID 1577804 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 12.0 g. of 4-carboxybenzaldehyde, 13.6 g. of N,N'-carbonyldiimidazole and 100 ml. of tetrahydrofuran is allowed to stand for one hour, then 9.4 ml. of piperidine is added. The reaction mixture is allowed to stand for 18 hours, then heated at reflux temperature for one hour. Water is added and the solvent is distilled off. Methylene chloride is added and the solution is washed with 25 ml. of concentrated hydrochloric acid, then with water then is dried over magnesium sulfate. The mother liquor is concentrated to yield p-piperidinocarbonylbenzaldehyde as an oil.

WORKUP

后处理

  1. additionA mixture of 12.0 g
  2. waitto stand for 18 hours
  3. temperatureheated
  4. temperatureat reflux temperature for one hour
  5. distillationthe solvent is distilled off
  6. additionMethylene chloride is added
  7. washthe solution is washed with 25 ml
  8. dry with materialof concentrated hydrochloric acid, then with water then is dried over magnesium sulfate
  9. concentrationThe mother liquor is concentrated