반응 #699684

ord-c1ef2b91c0084b979560fcc2f9fcf530

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타are heated overnight
  2. 2
    온도After cooling
  3. 3
    세척the solution is washed with water
  4. 4
    농축concentrated under reduced pressure
  5. 5
    기타the brown solid is chromatographed over silica gel using the system chloroform/ethyl acetate (4:1)

실험 절차

8.2 g (40 mmol) of 2-methyl-4-(4-fluorobenzylidene)-oxazol-5-one of Example (II-1) in 100 ml of toluene are heated overnight under reflux with 6.3 g (50 mmol) of 3,4,4-trifluorobut-3-enol, with the addition of 200 mg of 4-dimethylaminopyridine. After cooling, the solution is washed with water and concentrated under reduced pressure and the brown solid is chromatographed over silica gel using the system chloroform/ethyl acetate (4:1). 6.5 g (Yield 49% of theory) of 3,4,4-trifluorobut-3-enyl 3-(4-fluorophenyl)-2-acetylamino-prop-2-enoate of mp.: 116° are obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06004992uspto-grants-1999_12