HRID1796196

反应详情

EQUATION

反应方程式

HRID 1796196 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1-t-butoxycarbonyl-4-hydroxypiperidine (3.32 g), 2-chloro-4-nitrophenol (2.36 g) and triphenylphosphine (5.11 g) in dichloromethane (60 ml), diethyl azodicarboxylate (3.10 ml) was added dropwise with stirring under ice-cooling, and the resulting mixture was stirred at room temperature for 18 hours and then evaporated in vacuo. The residue obtained was purified by chromatography on a silica gel column using a mixed solvent of hexane and ethyl acetate (5:2) as the eluent to afford the title compound (3.90 g, yield: 76%) as a pale yellow solid.

WORKUP

后处理

  1. temperaturecooling
  2. stirringthe resulting mixture was stirred at room temperature for 18 hours
  3. customevaporated in vacuo
  4. customThe residue obtained
  5. customwas purified by chromatography on a silica gel column