HRID1042321
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
1,3-Dibenzyl-4-oxo-piperidine-3-carboxylic acid methyl ester, (2, R1B=H, Z=benzyl) (17.52 g, 51.92 mmol) was suspended in 150 mL of 6N HCl:MeOH (5:1) and the mixture was heated to reflux temperature with stirring for 48 h. After cooling the mixture was basified to pH 10 with 6N NaOH and extracted with 3×200 mL dichloromethane. The combined organics were dried (MgSO4) and concentrated to give 11.60 g of the title compound as a colorless oil, 80%. LC-MS: RT=0.38 min. (M+H)+ 280.
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureto reflux temperature
- temperatureAfter cooling the mixture
- extractionextracted with 3×200 mL dichloromethane
- dry with materialThe combined organics were dried (MgSO4)
- concentrationconcentrated