HRID379933

反应详情

EQUATION

反应方程式

HRID 379933 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

In 40 ml of dimethylformamide were dissolved 4.12 g (14.7 mmol) of 1-(tert-butoxycarbonyl)-4-(methanesulfonyloxy)piperidine, and 2.53 g (2.21 mmol) of potassium thioacetate were added to the solution, followed by stirring of the resulting mixture at 105° C. for 4 hours under nitrogen atmosphere. After cooling, the reaction mixture was diluted with ethyl acetate and washed with water and then a saturated aqueous NaCl solution, followed by evaporation of the solvent. The thus obtained residue was subjected to silica gel column chromatography and the fractions eluted with a mixed solvent of hexane-ethyl acetate (5:1) were collected to obtain 5.19 g (yield: 81%) of the title compound as an oil.

WORKUP

后处理

  1. additionwere added to the solution
  2. temperatureAfter cooling
  3. washwashed with water
  4. customa saturated aqueous NaCl solution, followed by evaporation of the solvent
  5. washthe fractions eluted with a mixed solvent of hexane-ethyl acetate (5:1)
  6. customwere collected