反応 #316237

ord-6d8b524bc66b41bb9f60440b806b2f5f

溶媒

反応条件

温度
140°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction solution was cooled to room temperature
  2. 2
    抽出the mixture was extracted with ethyl acetate
  3. 3
    洗浄The ethyl acetate layer was washed with water
  4. 4
    乾燥was dried over anhydrous sodium sulfate
  5. 5
    その他The solvent was removed by distillation under the reduced pressure
  6. 6
    その他the residue was purified by thin layer chromatography

実験手順

Dimethyl sulfoxide (2 ml) was added to 5,6,5′-trimethyl-[2,2′]bipyridin-3-ol (50 mg), 4-chloroquinoline (115 mg), and cesium carbonate (228 mg), and the mixture was stirred at 140° C. for 5 hr. The reaction solution was cooled to room temperature, water was then added to the reaction solution, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by thin layer chromatography using chloroform-methanol to give the title compound (57 mg, yield 72%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07560558B2uspto-grants-2009_07