تفاعل #9274

معادلة التفاعل

2-bromopyridine

1-butyne

→

title compound

المردود 84.3%

2-(1-Butynyl)pyridine

المردود 84.3%

المذيبات

diethylamine

ظروف التفاعل

المعالجة

1. 1
   أخرىAfter bubbling in nitrogen
2. 2
   استخلاصextraction
3. 3
   ترشيحThe insoluble portion was filtered out with celite
4. 4
   غسيلthe organic layer was washed with water and brine
5. 5
   تجفيفAfter drying over anhydrous magnesium sulfate and filtration
6. 6
   تركيزthe solvent was concentrated under reduced pressure
7. 7
   أخرىthe residue was purified by silica gel column chromatography

الإجراء التجريبي

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.

المصدر