反応 #6013

ord-f45c559759264321ac72a2b37dcee8d3

反応条件

温度
50°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄washed with dimethyl formamide
  2. 2
    その他The DMF is evaporated off under reduced pressure
  3. 3
    抽出An extraction with ether
  4. 4
    乾燥The organic phase is dried over sodium sulfate
  5. 5
    ろ過filtered
  6. 6
    その他The ether phase is evaporated to dryness under reduced pressure
  7. 7
    その他the product is recrystallized in petroleum ether

実験手順

0.06 mol of potassium carbonate and then 0.015 mol of 1-bromo-2-chloroethane are added to a solution of 0.015 mol of benzoselenazolinone in 30 cm3 of dimethylformamide. The mixture is heated to 50° C. with stirring for six hours. The inorganic precipitate is drained and then washed with dimethyl formamide. The DMF is evaporated off under reduced pressure and the residue is taken up with water. An extraction with ether is then carried out. The organic phase is dried over sodium sulfate and then filtered. The ether phase is evaporated to dryness under reduced pressure and the product is recrystallized in petroleum ether.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05246951uspto-grants-1993_09