반응 #1136369

ord-faaea11594c14f8b93ec86994ebbeeeb

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도at reflux until intermediate
  2. 2
    기타After reaction
  3. 3
    기타(18 hrs) it
  4. 4
    기타was brought to room temperature
  5. 5
    여과filtered

실험 절차

5-amino-3-((3-chloro-4-fluorophenyl)amino)-1H-pyrazole-4-carboxamide was then suspended in 8 mL EtOH and 4-hydroxybenzaldehyde (45 mg, 1 eq.) and piperidine (4-drops) were added. Stirred at reflux until intermediate was absent (HPLC). After reaction was complete (18 hrs) it was brought to room temperature and filtered to obtain 3-((3-chloro-4-fluorophenyl)amino)-5-((4-hydroxybenzylidene)amino)-1H-pyrazole-4-carboxamide as a yellow powder. Powder was washed with EtOH to remove any excess 4-hydroxybenzaldehyde. Product was allowed to dry under vacuum for 1 hr (147 mg, 53% yield).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09382237B2uspto-grants-2016_07