反応 #48832

ord-e9d217611dd942d58da602e9cc758320

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

2,4,5-Trifluorophenyl sulfonyl chloride (279 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 (169 mg). The material was used without further purification. 1H NMR δ (d6-DMSO): 3.35 (s, 3H), 7.87-8.01 (m, 2H).

出典

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