HRID238237
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureto reflux for 6 hr
- customthe solvent was removed in vacuo
- additionThe residue was diluted with water
- extractionextracted with EtOAc (300 mL×3)
- dry with materialthe organic layer was dried with Na2SO4
- concentrationconcentrated
- custompurified by column chromatography