HRID382790

反应详情

EQUATION

反应方程式

HRID 382790 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 13.5 g (SR)-1,4-dibenzyl-3-oxo-piperidine-4-carboxylic acid ethyl ester (38.4 mmol) in 20 ml ethanol were added 47.5 ml HCl (37%) and the yellow solution was refluxed for 48 h. The reaction mixture was cooled to 0° C. and NaOH was added until pH 8 was reached. The aqueous phase was extracted three times with ethyl acetate (200 ml) and the combined organic phases were washed with water (2×100 ml) and brine (2×100 ml). The organic phase was dried over MgSO4, filtrated and the solvent was removed under reduced pressure to give 9.8 g of the product (35 mmol, 91%) as a brown oil.

WORKUP

后处理

  1. temperaturethe yellow solution was refluxed for 48 h
  2. extractionThe aqueous phase was extracted three times with ethyl acetate (200 ml)
  3. washthe combined organic phases were washed with water (2×100 ml) and brine (2×100 ml)
  4. dry with materialThe organic phase was dried over MgSO4
  5. filtrationfiltrated
  6. customthe solvent was removed under reduced pressure