HRID238237

反应详情

EQUATION

反应方程式

HRID 238237 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-[1-(2-carbamoyl-phenylcarbamoyl)-ethyl]-piperidine-1-carboxylic acid tert-butyl ester (20 g, 0.05 mmol, crude from the last step) and MeONa (10 g, 0.19 mol) in MeOH (500 mL) was heated to reflux for 6 hr and the solvent was removed in vacuo. The residue was diluted with water and extracted with EtOAc (300 mL×3), the organic layer was dried with Na2SO4, concentrated and purified by column chromatography to afford the product (2 g, 5%).

WORKUP

后处理

  1. temperatureto reflux for 6 hr
  2. customthe solvent was removed in vacuo
  3. additionThe residue was diluted with water
  4. extractionextracted with EtOAc (300 mL×3)
  5. dry with materialthe organic layer was dried with Na2SO4
  6. concentrationconcentrated
  7. custompurified by column chromatography