反応 #72475
ord-bc1df6958e8c495a952b555eab578d2a
反応方程式
溶媒
反応条件
温度
42.5°CELSIUS
詳細条件
See reaction.notes.procedure_details.
後処理
- 1workup.ADDITIONwere added
- 2濃縮Then the mixture was concentrated in vacuo to half of its volume
- 3その他the product that precipitated
- 4ろ過was filtered off with suction
- 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.