반응 #8994

ord-fa30808a5c6741da93b67d37f1883a74

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The mixture is filtered
  2. 2
    기타the solvent is evaporated under reduced pressure
  3. 3
    기타to yield the crude product which
  4. 4
    기타is purified by recrystallisation from diethylether-hexane

실험 절차

A solution of 2-nitro-N-(4-bromo-3-trifluoromethylphenyl)benzamide (intermediate 1a; 32 g, 82 mmol) in methanol (1000 mL) is hydrogenated at atmospheric pressure over Raney nickel (6 g) at 21° C. The calculated amount of hydrogen is taken up after 7 hours. The mixture is filtered and the solvent is evaporated under reduced pressure to yield the crude product which is purified by recrystallisation from diethylether-hexane to give the title compound as a colourless crystalline solid, m.p. 142–144° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091224B2uspto-grants-2006_08