HRID1895989
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 mixture of the compound of Example 3 (0.076 g, 0.36 mmol), 4-bromoisoquinoline (0.064 g, 0.30 mmol), cesium carbonate (0.494 g, 1.5 mmol), 2,2′-bis(diphenylphosphino)-1,1′binaphthalene (0.011 g, 0.024 mmol), palladium(II)acetate (0.0027 mg, 0.012 mmol) in anhydrous and degassed toluene (3 mL) was heated at reflux under a nitrogen atmosphere for 18 h. The reaction mixture was cooled, poured into water and extracted with EtOAc. The combined organic layers were washed with brine, dried on Na2SO4 and evaporated to dryness in vacuo to afford a residue, which was purified by flash chromatography (CHCl3-1.4 N MeOH NH3 100:0.25) affording the title product (0.061 g).
WORKUP
后处理
- customdegassed toluene (3 mL)
- temperaturewas heated
- temperatureat reflux under a nitrogen atmosphere for 18 h
- temperatureThe reaction mixture was cooled
- additionpoured into water
- extractionextracted with EtOAc
- washThe combined organic layers were washed with brine
- customdried on Na2SO4
- customevaporated to dryness in vacuo
- customto afford a residue, which
- customwas purified by flash chromatography (CHCl3-1.4 N MeOH NH3 100:0.25)