反応 #74132

ord-f302bd22f2fc42149f1b3114c369e671

反応条件

温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出the product extracted with dichloromethane
  2. 2
    乾燥The organic phase was dried over sodium sulphate
  3. 3
    その他the solvent evaporated under reduced pressure
  4. 4
    その他2.4 g (86%) of the title compound crystallized from a mixture diethylether-diisopropylether

実験手順

2 g (6.3 mmol) of 4-iodo-3-(3-nitrophenyl)-1H-pyrazole were dissolved in 20 ml of dry dimethylformamide and 2.46 g (7.5 mmol) of cesium carbonate and 0.85 ml (6.3 mmol) of p-methoxybenzyl chloride were added successively. The reaction mixture was heated at 70° C. under stirring for 5 hours. Water was then added and the product extracted with dichloromethane. The organic phase was dried over sodium sulphate and the solvent evaporated under reduced pressure. 2.4 g (86%) of the title compound crystallized from a mixture diethylether-diisopropylether.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541575B2uspto-grants-2013_09