HRID272095

反应详情

EQUATION

反应方程式

HRID 272095 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 7.96 g of {(3S)-1-(tert-butoxycarbonyl)-3-piperidyl}methanol in 150 ml of chloroform, 3.4 ml of methanesulfonyl chloride and 6.7 ml of triethylamine were added under cooling with ice, followed by an hour's stirring at room temperature. The reaction liquid was distilled off under reduced pressure, diluted with ethyl acetate and saturated aqueous sodium bicarbonate solution was added, followed by 1.5 hours' stirring. Thereafter the reaction liquid was successively washed with water and saturated brine and dried over anhydrous magnesium sulfate. Distilling the solvent off, 10.50 g of the title compound was obtained.

WORKUP

后处理

  1. temperatureunder cooling with ice
  2. waitfollowed by an hour
  3. customThe reaction liquid
  4. distillationwas distilled off under reduced pressure
  5. additiondiluted with ethyl acetate and saturated aqueous sodium bicarbonate solution
  6. additionwas added
  7. stirring' stirring
  8. customThereafter the reaction liquid
  9. washwas successively washed with water and saturated brine
  10. dry with materialdried over anhydrous magnesium sulfate
  11. distillationDistilling the solvent off, 10.50 g of the title compound
  12. customwas obtained