반응 #1259748

ord-d278318a0b974579b4a3a2b6c361627e

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도under reflux for 2 hours
  2. 2
    농축concentrated under reduced pressure
  3. 3
    세척washed with water, brine
  4. 4
    건조dried with Na2SO4
  5. 5
    농축concentrated under reduced pressure
  6. 6
    기타The resulting crude product was purified by column chromatography (95% CH2Cl2, 4% MEOH, 1% Et3N)

실험 절차

2-Furan-2-yl-5-methanesulfonyl-[1,2,4]triazolo[1,5-a][1,3,5]triazin-7-ylamine (0.7 mmol, 1 eq.; see J. Chem. Soc. Perkin Trans. 1, 801 (1995)) and 2,5-diaza-bicyclo[2.2.1]heptane (5 eq.) were suspended in 10 mL of CH3CN. The mixture was stirred under reflux for 2 hours. It was then cooled to room temperature and concentrated under reduced pressure. The residue was taken up in CH2Cl2 and washed with water, brine, dried with Na2SO4, and concentrated under reduced pressure. The resulting crude product was purified by column chromatography (95% CH2Cl2, 4% MEOH, 1% Et3N) to afford 5-(2,5-diaza-bicyclo[2.2.1]hept-2-yl)-2-furan-2-yl-[1,2,4]triazolo[1,5-a][1,3,5]triazin-7-ylamine.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07834014B2uspto-grants-2010_11