تفاعل #490111

ord-d3dbf29455954ae3a7d53f501695c330

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةto warm to room temperature
  2. 2
    workup.STIRRINGstir 18 h
  3. 3
    أخرىThe reaction mixture was quenched with sat. NaHCO3 (aq)
  4. 4
    workup.ADDITIONdiluted with water and EtOAc
  5. 5
    ترشيحAn insoluble solid was collected by filtration

الإجراء التجريبي

A mixture of 8-bromo-6-chloroimidazo[1,2-b]pyridazine (272 mg, 1.17 mmol, Eq: 1.00) and (6-aminopyridin-3-yl)(morpholino)methanone (255 mg, 1.23 mmol, Eq: 1.05) in DMF (10.0 ml) was cooled to 0° C. To this reaction mixture was added sodium hydride (150 mg, (60% in mineral oil), 3.74 mmol, Eq: 3.2). The reaction was allowed to stir at 0° C. for 10 minutes and then allowed to warm to room temperature and stir 18 h. The reaction mixture was quenched with sat. NaHCO3 (aq) and diluted with water and EtOAc. An insoluble solid was collected by filtration to give [6-(6-chloro-imidazo[1,2-b]pyridazin-8-ylamino)-pyridin-3-yl]-morpholin-4-yl-methanone (420 mg, 99%). LC/MS-ESI observed [M+H]+ 358.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08742098B2uspto-grants-2014_06