反応 #367284

ord-cffe62231e314e2db4be994c382c6749

反応方程式

[F-].[Na+]
sodium fluoride
CCOC(=O)C(=CNC1CC1)C(=O)c1cc(F)c(F)c(F)c1F
ethyl 2-(2,3,4,5-tetrafluorobenzoyl)-3-cyclopropylaminoacrylate
CCOC(=O)c1cn(C2CC2)c2c(F)c(F)c(F)cc2c1=O
ethyl 1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate
収率 90.0%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度under reflux for 2 hours
  2. 2
    workup.ADDITIONwhile hot, poured onto ice
  3. 3
    ろ過The precipitate is filtered off with suction
  4. 4
    洗浄thoroughly washed with water
  5. 5
    乾燥dried over calcium chloride at 100° C. in vacuo

実験手順

21.2 g of sodium fluoride are added to a solution of 107.8 g of ethyl 2-(2,3,4,5-tetrafluorobenzoyl)-3-cyclopropylaminoacrylate in 400 ml of anhydrous dimethylformamide. The reaction mixture is then stirred under reflux for 2 hours and, while hot, poured onto ice. The precipitate is filtered off with suction, thoroughly washed with water and dried over calcium chloride at 100° C. in vacuo. 91.2 g of ethyl 1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate of melting point 167°-168° C. are obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04588726uspto-grants-1986_05