HRID657647
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customclose to 60° C. for one hour
- customat room temperature overnight and finally 6 h at a temperature close to 90° C
- concentrationThe solution is concentrated under reduced pressure
- dissolutionredissolved in dichloromethane
- filtrationfiltered