반응 #610280

ord-7663a71618584c9f9ac14ad722f6976f

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The reaction mixture was filtered
  2. 2
    workup.ADDITIONdiluted with NaCl solution
  3. 3
    추출extracted with EtOAc
  4. 4
    기타The organic layer was purified
  5. 5
    세척by eluting through an SCX-2 column
  6. 6
    세척eluting with 0-4% MeOH/EtOAc

실험 절차

A suspension of 6-bromo-2-methoxypyridin-3-amine (96 mg, 0.473 mmol), 1,2-dimethyl-1H-imidazole (91 mg, 0.946 mmol), Pd(OAc)2 (4.3 mg, 0.019 mmol), KOAc (93 mg, 0.95 mmol) in DMA (3 mL) was stirred at 1500 under microwave irradiation for 8 hours. The reaction mixture was filtered, diluted with NaCl solution and extracted with EtOAc. The organic layer was purified by eluting through an SCX-2 column using 2M NH3/MeOH followed by Biotage silica gel column chromatography eluting with 0-4% MeOH/EtOAc to give the title compound as pink solid (17 mg, 16%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09334286B2uspto-grants-2016_05