反応 #72475

ord-bc1df6958e8c495a952b555eab578d2a

溶媒

反応条件

温度
42.5°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwere added
  2. 2
    濃縮Then the mixture was concentrated in vacuo to half of its volume
  3. 3
    その他the product that precipitated
  4. 4
    ろ過was filtered off with suction
  5. 5
    洗浄washed with a small amount of toluene

実験手順

25.90 g (0.07 mol) of 2-(4-chloro-phenylsulfonylamino)-4,5-dimethoxy-benzoic acid were mixed with 75 ml of toluene, 17.30 g (0.08 mot) of phosphorus pentachloride were added and the mixture was stirred at 40-45° C. for 2.5 h. Then the mixture was concentrated in vacuo to half of its volume and the product that precipitated was filtered off with suction and washed with a small amount of toluene. 25.30 g (93%) of 2-(4-chloro-phenylsulfonylamino)-4,5-dimethoxy-benzoyl chloride having a melting point of 175-177° C. were obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541410B2uspto-grants-2013_09