HRID2407495

反应详情

EQUATION

反应方程式

HRID 2407495 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 1-benzylpiperidine-3,3-dicarboxylic acid 3,3-dibenzyl ester (19.6 g 41.8 mmol) and sodium carbonate (5.1 g, 48.1 mmol) in chloroform cooled with a water/ice bath, is added 2,2,2-trichloroethyl chloroformate (11 g, 51.8 mmol). The mixture is stirred overnight at room temperature and concentrated under reduced pressure. The residue is dissolved in diethyl oxide, washed with water, dried over magnesium sulphate and concentrated under reduced pressure to give piperidine-1,3,3-tricarboxylic acid 1-(2,2,2-trichloroethyl) 3,3-dibenzyl ester which cristallizes upon standing.

WORKUP

后处理

  1. temperaturecooled with a water/ice bath
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThe residue is dissolved in diethyl oxide
  4. washwashed with water
  5. dry with materialdried over magnesium sulphate
  6. concentrationconcentrated under reduced pressure