HRID602447

反应详情

EQUATION

反应方程式

HRID 602447 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of ethyl {cis-1-benzyl-5-[(tert-butoxycarbonyl)amino]piperidin-2-yl}acetate (2.0 g, 5.31 mmol, step 6 of Example 1) and 10% hydrochloric acid in methanol was stirred at room temperature for 20 h. The mixture was concentrated under reduced pressure. The resulting residue was dissolved in dichloromethane/methanol (10/1, 10 mL). The solution was filtered through amine-silica gel washing with dichloromethane/methanol (10/1, 200 mL). The filtrate was concentrated under reduced pressure to give 1.65 g (quant.) of the title compound as a brown amorphous solid.

WORKUP

后处理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. dissolutionThe resulting residue was dissolved in dichloromethane/methanol (10/1, 10 mL)
  3. filtrationThe solution was filtered through amine-silica gel washing with dichloromethane/methanol (10/1, 200 mL)
  4. concentrationThe filtrate was concentrated under reduced pressure