반응 #160526

ord-d523f99817fb4c26aa9722aefbfb32cf

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출this mixture was extracted with diethyl ether
  2. 2
    세척This organic layer was washed with brine
  3. 3
    건조dried over anhydrous magnesium sulfate
  4. 4
    여과filtered
  5. 5
    기타The solvent was removed under reduced pressure
  6. 6
    세척This residue was washed with ethanol

실험 절차

A suspension of 1,4-difluoro-2-methyl-5-nitrobenzene (1.00 g), cyanoacetic acid benzyl ester (1.01 g) and potassium carbonate (1.76 g) in N,N-dimethylformamide (20.0 mL) was stirred at 60° C. for 1 day. To this reaction mixture was added 1 mol/L hydrochloric acid (25.4 mL), and this mixture was extracted with diethyl ether. This organic layer was washed with brine, and dried over anhydrous magnesium sulfate, and filtered. The solvent was removed under reduced pressure. This residue was washed with ethanol to give the title compound (1.54 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08829040B2uspto-grants-2014_09