HRID1743258

反应详情

EQUATION

反应方程式

HRID 1743258 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6.9 g of 4-hydroxypiperidine were dissolved in 150 ml of THF. 19.4 g of 2-(trimethylsilyl)ethyl 4-nitrophenyl carbonate and 11.9 ml of N,N-diisopropylethylamine were successively added thereto. The mixture was stirred at room temperature for 1 h and then the solvent was removed in vacuo. The residue was taken up in 400 ml of ethyl acetate and washed once with 200 ml of 0.5 N HCl and twice with 200 ml of 1 N NaOH each time. The organic phase was dried with MgSO4, the solvent was removed in vacuo, and the residue was purified by chromatography on silica gel.

WORKUP

后处理

  1. customthe solvent was removed in vacuo
  2. washwashed once with 200 ml of 0.5 N HCl and twice with 200 ml of 1 N NaOH each time
  3. dry with materialThe organic phase was dried with MgSO4
  4. customthe solvent was removed in vacuo
  5. customthe residue was purified by chromatography on silica gel