반응 #693081

ord-3684360a7a85498ab746982dbb10aa0e

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The reaction mixture is evaporated to dryness
  2. 2
    기타the residue partitioned between dichloromethane and water
  3. 3
    추출The aqueous phase is extracted twice with dichloromethane
  4. 4
    세척The organic layers are washed with brine
  5. 5
    건조dried over MgSO4
  6. 6
    여과filtered
  7. 7
    기타evaporated

실험 절차

A mixture of 5,8-dibromo-[1,2,4]triazolo[1,5-a]pyrazine (2 g, 7.20 mmol), 4-(4-methyl-piperazin-1-yl)-phenylamine (1.65 g, 8.64 mmol) and N-ethyldiisopropyl-amine (1.5 mL, 8.64 mmol) is heated at 80° C. in 2-propanol (50 mL) for 8 hours. The reaction mixture is evaporated to dryness and the residue partitioned between dichloromethane and water. The aqueous phase is extracted twice with dichloromethane. The organic layers are washed with brine, dried over MgSO4, filtered and evaporated to furnish the title compound (1.41 g) as a grey solid. 1H-NMR (400 MHz, d6-DMSO) δ (ppm) 2.27 (3H, s), 2.54 (4H, m), 3.14 (4H, m), 6.97 (2H, d), 7.80 (2H, d), 7.87 (1H, s), 8.72 (1H, s), 9.92 (1H, br s). LCMS: Rt 2.07 min (77.4%), m/z (APCI) 388 (M+H)+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07915256B2uspto-grants-2011_03