반응 #1860835

ord-89ba40aa77ee467e87e502affb9f25f8

반응 조건

온도
70°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타After reaction for 72 h
  2. 2
    추출Extraction
  3. 3
    여과with ethyl acetate/water, filtration of the organic phase through a Whatman
  4. 4
    여과filter
  5. 5
    기타evaporation of the organic phase

실험 절차

To a stirred solution of 4.96 g (11.06 mmol) N-cyclopropyl-4-[6-(3-fluorophenoxy)-8-(methylsulfanyl)imidazo[1,2-b]pyridazin-3-yl]-2-methylbenzamide which was prepared according to intermediate example 486b in DMF (250 mL) were added 20.4 g (33.18 mmol) oxone in one portion at rt. After reaction for 72 h, further 30 g (55 mmol) oxone are added and the mixture is heated at 70° C. for one hour. Extraction with ethyl acetate/water, filtration of the organic phase through a Whatman filter and evaporation of the organic phase yielded the crude product (4.96 g, 93%) which was used without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09255100B2uspto-grants-2016_02