HRID2059894

反应详情

EQUATION

反应方程式

HRID 2059894 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 4-(1-(4-methoxy-2,6-dimethylphenylsulfonyl)piperidin-2-yl)butanoic acid methyl ester (1.65 g, 4.3 mmol) was dissolved in water (10 ml) and methanol (35 ml) and lithium hydroxide (0.3 g, 12.9 mmol) was added. The mixture was stirred for 3 d at room temperature, then methanol was distilled off under vacuum and ethyl acetate (50 ml) and HCl solution (1 mol/l, 10 ml) added to the residue. Phase separation, extraction with ethyl acetate (2×50 ml), the combined organic phases were dried over sodium sulfate and concentrated to small volume under vacuum. Yield: 1.56 g (98%)

WORKUP

后处理

  1. distillationmethanol was distilled off under vacuum and ethyl acetate (50 ml) and HCl solution (1 mol/l, 10 ml)
  2. additionadded to the residue
  3. customPhase separation, extraction with ethyl acetate (2×50 ml)
  4. dry with materialthe combined organic phases were dried over sodium sulfate
  5. concentrationconcentrated to small volume under vacuum