HRID1583319

反应详情

EQUATION

反应方程式

HRID 1583319 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7.9 g. of α-ethyl-α-(3-chlorphenyl)-4-hydroxybenzyl alcohol, 14 g. of anhydrous potassium carbonate and 6.6 g. of N-(3-chloropropyl)-piperidine hydrochloride in 80 ml. of methyl isobutyl ketone are boiled under moderate reflux for three hours. The solvent is distilled off under reduced pressure, to the residue water is added and it is extracted with benzene. The benzene phase is washed with an aqueous potassium hydroxide solution and subsequently with water, dried over anhydrous magnesium sulfate, and evaporated to dryness in vacuo. Crystallization of the residue from n-hexane yields 8.6 g. of the title compound, melting at 80° to 81° C.

WORKUP

后处理

  1. temperatureunder moderate reflux for three hours
  2. distillationThe solvent is distilled off under reduced pressure, to the residue water
  3. additionis added
  4. extractionit is extracted with benzene
  5. washThe benzene phase is washed with an aqueous potassium hydroxide solution and subsequently with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customevaporated to dryness in vacuo
  8. customCrystallization of the residue from n-hexane
  9. customyields 8.6 g