반응 #332487

ord-dab7557d28b94e99a376ef3f67a047bb

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도while maintaining the temperature below 50° C
  2. 2
    추출The mixture was extracted with ethyl acetate
  3. 3
    세척washed with brine
  4. 4
    건조dried over anhydrous magnesium sulfate
  5. 5
    여과filtered
  6. 6
    기타dried

실험 절차

3,4-difluoro-nitrobenzene (100 g, 0.63 mol) was added dropwise to morpholine (60 g, 0.69 mol) and triethylamine (70 g, 0.69 mol) in ethyl acetate (300 mL) within 1 hour while maintaining the temperature below 50° C. The mixture is stirred at 45˜50° C. for 10 hours until the completion of the reaction. The mixture was extracted with ethyl acetate, washed with brine and dried over anhydrous magnesium sulfate, filtered, dried, to provide 138 g of yellow solid in 97% yield.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08658789B2uspto-grants-2014_02