HRID485629

反应详情

EQUATION

反应方程式

HRID 485629 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 7 liters of toluene were added 695 grams (4.4M) of ethyl nipecotate, 1304 grams (4.8M) of p-methoxybenzyl trichloroacetate, and 660 grams (4.8M) of potassium carbonate. The mixture was refluxed for 72 hours under a nitrogen atmosphere after which it was cooled, and the solvent was removed in vacuo. The resulting oil was dissolved in chloroform, and the solution was washed with 10% aqueous potassium carbonate followed by 10% aqueous hydrochloric acid. The solution then was dried over sodium sulfate and concentrated in vacuo. The resulting oil was triturated with ethyl ether, yielding 783 grams of the title compound as a solid.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 72 hours under a nitrogen atmosphere after which it
  2. temperaturewas cooled
  3. customthe solvent was removed in vacuo
  4. dissolutionThe resulting oil was dissolved in chloroform
  5. washthe solution was washed with 10% aqueous potassium carbonate
  6. dry with materialThe solution then was dried over sodium sulfate
  7. concentrationconcentrated in vacuo
  8. customThe resulting oil was triturated with ethyl ether