反応 #8473
ord-68e35b96105c48e0ba0ea364160d7487
反応方程式
反応条件
温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度The mixture was cooled to ambient temperature
- 2温度heated
- 3温度at reflux temperature for 18 hours
- 4温度The mixture was cooled to ambient temperature
- 5その他evaporated to dryness
- 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).