HRID45987

反应详情

EQUATION

反应方程式

HRID 45987 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The ethyl 2-(1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-2-yl)acetate (10.45 g, 27.5 mmol) was dissolved in a mixture of methanol (150 ml), dioxane (40 ml) and aqueous NaOH solution (4 M, 41.3 ml, 165.2 mmol, 6 eq.) and the solution was stirred overnight When the reaction had ended (TLC control, MC/methanol 95:5), the solution was concentrated. The crude product was taken up in ethyl acetate (600 ml) and the mixture was . . . with KHSO4 solution (0.5 M, 600 ml). The aqueous phase was extracted once more with ethyl acetate (100 ml) and the combined organic phases were washed with sat. NaCl solution (500 ml), dried over Na2SO4 and concentrated. Yield: 9.4 g, 97%.

WORKUP

后处理

  1. concentrationthe solution was concentrated
  2. extractionThe aqueous phase was extracted once more with ethyl acetate (100 ml)
  3. washthe combined organic phases were washed with sat. NaCl solution (500 ml)
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated