反応 #492367

ord-bf921c0c8e4e4efc98e1e80d12b92bc1

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度After 70 min the resulting mixture was cooled to room temperature
  2. 2
    乾燥dried (Na2SO4)
  3. 3
    濃縮concentrated
  4. 4
    その他purified via column chromatography

実験手順

2-bromo-4,6-bis(trifluoromethyl)benzaldehyde (100 mg, 0.31 mmol), ethyl 3-(5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)picolinamido)propanoate (119 mg, 0.34 mmol), Pd(dppf)Cl2 (23 mg, 0.03 mmol), and 2M K2CO3 (0.31 mL, 0.62 mmol), were dissolved in 1,4-dioxane (1.0 mL) and heated to 100° C. After 70 min the resulting mixture was cooled to room temperature, diluted with DCM, dried (Na2SO4), concentrated and purified via column chromatography to yield the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08748624B2uspto-grants-2014_06