HRID2263048

反应详情

EQUATION

反应方程式

HRID 2263048 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 tert-butyl 3-aminopiperidine-1-carboxylate (1.00 g, 4.99 mmol) and pyridine (489 ml, 5.99 mmol) in tetrahydrofuran (16 ml) was added, under ice-cooling, 2,2,2-trichloroethyl chloroformate (0.829 ml, 5.99 mmol), and the mixture was stirred at room temperature for 1 hour. Water was poured to the reaction mixture, and the resulting solution was extracted with ethyl acetate. The extract was introduced to water and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to give 867 mg (46.2%) of the desired product as an oil.

WORKUP

后处理

  1. temperaturecooling
  2. extractionthe resulting solution was extracted with ethyl acetate
  3. additionThe extract was introduced to water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationThe solvent was distilled off under reduced pressure