反応 #48830

ord-b692961d75f642889f4ac786d8c9eff8

反応条件

温度
150°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to cool
  2. 2
    温度heated to 150° C. for 300 seconds
  3. 3
    温度to cool
  4. 4
    その他was removed by filtration
  5. 5
    その他dried in vacuo

実験手順

2-Chloro-4,5-difluorobenzenesulfonyl chloride (300 mg) was added to a solution of sodium sulfite (306 mg) and sodium bicarbonate (153 mg) in water (4 mL). The mixture was heated to 150° C. in a sealed microwave vial for 400 seconds and allowed to cool. The mixture was treated with bromoacetic acid (253 mg) in water (1 mL), and heated to 150° C. for 300 seconds then allowed to cool, following which the precipitate was removed by filtration and dried in vacuo to give the desired compound (132 mg). The material was used without further purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07745475B2uspto-grants-2010_06