反应 #11546
ord-058da2b8cb024016b60ad8909917c9ed
反应方程式
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度the mixture was refluxed for 1.5 hours
- 2过滤Then, the solid was filtered out
- 3洗涤washed with toluene and 2-propanol successively
- 4浓缩The filtrate was concentrated under reduced pressure
- 5其他the residue was purified by basic silica gel column chromatography
- 6过滤the resulting solid was filtered off with diisopropyl ether
实验过程
Ethylenediamine (10.4 ml, 155 mmol) was added to 4-bromopyridine hydrochloride (3.00 g, 15.5 mmol) under a nitrogen atmosphere, and the mixture was refluxed for 1.5 hours. The temperature was cooled to room temperature, potassium carbonate (8.57 g, 62.0 mmol) was added to the reaction mixture, and the whole was stirred for 10 minutes. Then, the solid was filtered out and washed with toluene and 2-propanol successively. The filtrate was concentrated under reduced pressure, the residue was purified by basic silica gel column chromatography, and the resulting solid was filtered off with diisopropyl ether to give 1.63 g (77%) of the titled compound as a pale yellow solid.