反应 #11546

ord-058da2b8cb024016b60ad8909917c9ed

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度the mixture was refluxed for 1.5 hours
  2. 2
    过滤Then, the solid was filtered out
  3. 3
    洗涤washed with toluene and 2-propanol successively
  4. 4
    浓缩The filtrate was concentrated under reduced pressure
  5. 5
    其他the residue was purified by basic silica gel column chromatography
  6. 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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07098226B2uspto-grants-2006_08