HRID657647

反应详情

EQUATION

反应方程式

HRID 657647 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A degazed solution of 1-{3-[(4′-bromobiphenyl-4-yl)oxy]propyl}piperidine (2.8 g), triethylamine (2.8 mL), tri(o-tolyl)phosphine (365 mg), palladium acetate (170 mg) and ethyl acrylate (2.9 mL) in acetonitrile (5 mL) is stirred at a temperature close to 60° C. for one hour, then at room temperature overnight and finally 6 h at a temperature close to 90° C. The solution is concentrated under reduced pressure, redissolved in dichloromethane, filtered and chromatographied over silica gel to give 1.3 g of 1-(3-{[4′-(2-ethoxycarbonylethen-1-yl)biphenyl-4-yl]oxy}propyl)piperidine.

WORKUP

后处理

  1. customclose to 60° C. for one hour
  2. customat room temperature overnight and finally 6 h at a temperature close to 90° C
  3. concentrationThe solution is concentrated under reduced pressure
  4. dissolutionredissolved in dichloromethane
  5. filtrationfiltered