HRID1643474

反应详情

EQUATION

反应方程式

HRID 1643474 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

PBr3 (2.64 mmol, 1.5 eq) was added to a solution of 3-(1-(4-methoxy-2,6-dimethylphenylsulfonyl)piperidin-2-yl)propan-1-ol (1.76 mmol, 1 eq) in DMF (6 ml) at 0° C. and the mixture was stirred for 30 min. Water (20 ml) was subsequently added and the mixture was extracted with ethyl acetate. The organic phase was washed with water and sat. sodium chloride solution, dried (Na2SO4) and concentrated in vacuo. The crude product obtained in this way was purified by column chromatography (silica gel). Yield: 25%

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic phase was washed with water and sat. sodium chloride solution
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated in vacuo