反応 #492364

ord-cc16595dd6474e028164fbe3a12a1717

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 4 h 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-chloro-6-methylbenzaldehyde (156 mg, 1.01 mmol), ethyl 3-(5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)picolinamido)propanoate (434 mg, 1.25 mmol), Pd(PPh3)4 (58 mg, 0.05 mmol), and 2M K3PO4 (aq) (1.0 mL, 2.00 mmol) were dissolved in 1,4-dioxane (3.0 mL) and heated to 100° C. After 4 h 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