反应 #9274

反应方程式

2-bromopyridine

1-butyne

→

title compound

收率 84.3%

2-(1-Butynyl)pyridine

收率 84.3%

溶剂

diethylamine

反应条件

后处理

1. 1
   其他After bubbling in nitrogen
2. 2
   萃取extraction
3. 3
   过滤The insoluble portion was filtered out with celite
4. 4
   洗涤the organic layer was washed with water and brine
5. 5
   干燥After drying over anhydrous magnesium sulfate and filtration
6. 6
   浓缩the solvent was concentrated under reduced pressure
7. 7
   其他the residue was purified by silica gel column chromatography

实验过程

After dissolving 2-bromopyridine (50 g) in diethylamine (500 mL) and adding dichlorobis(triphenylphosphine)palladium (II) (2.2 g) and copper iodide (0.3 g), the mixture was stirred at room temperature for 4 hours while introducing 1-butyne (100 g) as a gas. After bubbling in nitrogen, extraction was performed with ethyl acetate. The insoluble portion was filtered out with celite, and then the organic layer was washed with water and brine. After drying over anhydrous magnesium sulfate and filtration, the solvent was concentrated under reduced pressure, the residue was purified by silica gel column chromatography, and the title compound (35 g) was obtained from the n-hexane:ethyl acetate (5:1) fraction as a brown oil.

来源