HRID540642

反应详情

EQUATION

反应方程式

HRID 540642 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture consisting of 42 mg of 4-[(E)-2-(5-bromopyridin-2-yl)vinyl]-2-methyloctahydropyrrolo[3,4-a]indolizine-1,3-dione (from Example 6, racemic mixture 1), 2.5 mg of tetrakis(triphenylphosphine)palladium(0), 25 mg of 3-trifluoromethylphenylboronic acid, 37 mg of potassium carbonate, 1.5 ml of toluene, 0.3 ml of ethanol and 0.75 ml of water is stirred at 100° C. for 5 h. After cooling, the mixture is taken up in 20 ml of water and the product is extracted by shaking with 20 ml of ethyl acetate. After drying and concentration of the organic phase, an oil is obtained. The crude product is purified by column chromatography (silica gel, MeOH:DCM=1:99).

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionthe product is extracted
  3. stirringby shaking with 20 ml of ethyl acetate
  4. customAfter drying
  5. customconcentration of the organic phase, an oil is obtained
  6. customThe crude product is purified by column chromatography (silica gel, MeOH:DCM=1:99)