HRID1777359

反应详情

EQUATION

反应方程式

HRID 1777359 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A solution of sodium hydroxide (0.1 g, 0.0023 mol) and potassium hydroxide (85% assay, 0.13 g, 0.0020 mol) in demineralized water (2 mL) is added to a solution of 4-methyl-1-{4-[5-(3-chloro-4-cyclohexylphenyl)-[1,2,4]-oxadiazol-3-yl]benzyl}piperidine-4-carboxylic acid ethyl ester (0.3 g, 0.00057 mol) in tetrahydrofuran and ethanol (14 mL, 1:1). The reaction mixture is heated under reflux (80° C.) for 2 hrs. It is then concentrated under reduced pressure to give a crude residue which is dissolved in demineralized water (10 mL) and acidified to pH˜4-5 with 20% aqueous acetic acid solution. The resultant solid is filtered, dried and washed with acetone (2×10 mL). Solid is dried under vacuum to get 1-{4-[5-(3-chloro-4-cyclohexylphenyl)-[1,2,4]-oxadiazol-3-yl]benzyl}4-methyl piperidine-4-carboxylic acid.

WORKUP

后处理

  1. temperatureThe reaction mixture is heated
  2. concentrationIt is then concentrated under reduced pressure
  3. customto give a crude residue which
  4. filtrationThe resultant solid is filtered
  5. customdried
  6. washwashed with acetone (2×10 mL)
  7. customSolid is dried under vacuum