HRID1506191

反应详情

EQUATION

反应方程式

HRID 1506191 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Crude methyl rac-(3R,4R)-1-benzyl-4-methylpiperidin-3-ylcarbamate (2.3 g) in concentrated hydrochloric acid (15 mL) was refluxed for one day under heating and allowed to cool to room temperature. The hydrochloric acid was removed under reduced pressure, and the reaction mixture was partitioned between chloroform and saturated aqueous sodium chloride. The aqueous layer was basified with saturated aqueous sodium carbonate and extracted with ethyl acetate twice, and the organic layers were combined, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting brown oil (4.94 g) containing the title compound was used for the next step without further purification.

WORKUP

后处理

  1. temperatureunder heating
  2. customThe hydrochloric acid was removed under reduced pressure
  3. customthe reaction mixture was partitioned between chloroform and saturated aqueous sodium chloride
  4. extractionextracted with ethyl acetate twice
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. additionThe resulting brown oil (4.94 g) containing the title compound
  8. customwas used for the next step without further purification