HRID1042321

反应详情

EQUATION

反应方程式

HRID 1042321 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe mixture was heated
  2. temperatureto reflux temperature
  3. temperatureAfter cooling the mixture
  4. extractionextracted with 3×200 mL dichloromethane
  5. dry with materialThe combined organics were dried (MgSO4)
  6. concentrationconcentrated