HRID2388654

反应详情

EQUATION

反应方程式

HRID 2388654 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A 6 M aqueous NaOH solution (200 ml, 1.200 mmol) was added to a solution of tert-butyl 2-((1-(4-methoxy-2,6-dimethylphenylsulfonyl)piperidin-2-yl)methoxy)-acetate (26.8 g, 62.7 mmol) in THF (200 ml) and methanol (200 ml) and the reaction was stirred at room temperature for 1 hour. The organic solvents were then distilled off and 6 M aqueous HCl (210 ml) was added to the residue at 0° C. The aqueous phase was extracted with methylene chloride (200 ml) and ethyl acetate (200 ml). The combined organic phases were dried with Na2SO4, filtered and concentrated in vacuo. The residue obtained was codistilled twice with diisopropyl ether. The yield was 21.92 g (94%).

WORKUP

后处理

  1. distillationThe organic solvents were then distilled off
  2. addition6 M aqueous HCl (210 ml) was added to the residue at 0° C
  3. extractionThe aqueous phase was extracted with methylene chloride (200 ml) and ethyl acetate (200 ml)
  4. dry with materialThe combined organic phases were dried with Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue obtained