반응 #367284

ord-cffe62231e314e2db4be994c382c6749

반응 방정식

[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
수율 90.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도under reflux for 2 hours
  2. 2
    workup.ADDITIONwhile hot, poured onto ice
  3. 3
    여과The precipitate is filtered off with suction
  4. 4
    세척thoroughly washed with water
  5. 5
    건조dried over calcium chloride at 100° C. in vacuo

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04588726uspto-grants-1986_05