반응 #1012770

ord-fb1db4f3956343f1accf8cd96197d578

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출the mixture was extracted with ethyl acetate (3×200 mL)
  2. 2
    여과The organic phase was filtered
  3. 3
    기타evaporated
  4. 4
    기타the residue was recrystallized from MeOH/water

실험 절차

To a stirred solution of 6-bromo-3-iodo-8-methanesulfonyl-imidazo[1,2-a]pyrazine (5.08 g, 12.64 mmol) in NMP (100 mL) was added 3.77 mL isobutylamine (2.77 g, 37.90 mmol, 3 eq) in one portion at rt. After stirring for 2 h at rt, 500 mL water was added and the mixture was extracted with ethyl acetate (3×200 mL). The organic phase was filtered, evaporated and the residue was recrystallized from MeOH/water to yield 3.87 g (77.52%) (6-bromo-3-iodo-imidazo[1,2-a]pyrazin-8-yl)-isobutyl-amine: 1H-NMR (300 MHz, d6-DMSO): δ=8.09 (1H, tr), 7.60 (1H, s), 7.54 (1H, s), 3.19 (2H, dd), 1.95 (1H, m), 0.85 (6H, d) ppm.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09284317B2uspto-grants-2016_03