反応 #8473

ord-68e35b96105c48e0ba0ea364160d7487

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture was cooled to ambient temperature
  2. 2
    温度heated
  3. 3
    温度at reflux temperature for 18 hours
  4. 4
    温度The mixture was cooled to ambient temperature
  5. 5
    その他evaporated to dryness
  6. 6
    その他The residue was crystallized

実験手順

The product of Step A (1.8 g) in dry acetonitrile (40 mL) was treated sequentially with tetrakis(triphenylphosphine)palladium(0) (0.1 g), triethylamine (1.27 g), and CuI (10 mg) then heated at 60° C. for 30 minutes. The mixture was cooled to ambient temperature, treated with 3-butyn-1-ol (0.361 g) and heated at reflux temperature for 18 hours. The mixture was cooled to ambient temperature and evaporated to dryness. The residue was crystallized, twice, from acetone to afford the title compound (1.02 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07087757B2uspto-grants-2006_08