HRID606754

反应详情

EQUATION

反应方程式

HRID 606754 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 3-trimethylstannyl-5-carboxyethylpyridine (0.298 g, 0.949 mmol) and 4-(1-bromo-1-phenyl-methylene)-piperidine-1-carboxylic acid tert-butyl ester (0.334 mL, 0.949 mmol) in dry THF (5 mL) was degassed with a stream of Ar bubbles for 10 min. To this solution was added bis(triphenylphosphine)palladium dichloride (0.033 g, 0.047 mmol) and then the reaction vessel was sealed and the mixture was heated at 90° C. (oil bath temperature) for 16 h. The cooled mixture was then evaporated to dryness and the residue chromatographed (SiO2/hexane-EtOAc, 7:3) to give the title compound (0.294 g, 73%) as a clear yellow oil:

WORKUP

后处理

  1. customwas degassed with a stream of Ar bubbles for 10 min
  2. customthe reaction vessel was sealed
  3. customThe cooled mixture was then evaporated to dryness
  4. customthe residue chromatographed (SiO2/hexane-EtOAc, 7:3)