반응 #479609

ord-32fc6db824284f9f91ed2dd5ed977606

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The dark red reaction
  2. 2
    여과filtered
  3. 3
    농축concentrated to dryness
  4. 4
    기타The residue was purified by Biotage
  5. 5
    세척eluting with 3:1 to 2:1 DCM/EtOAc mixture

실험 절차

Into a 0° C. solution of N-(3-methoxycarbonylphenyl) pyrid-3-ylmethylamine (204 g, 0.842 mole, 1 eq) in dichloroethane (3610 mL) and pyridine (1775 mL) was added ethanesulfonyl chloride (114 mL, 1.2 mole, 1.43 eq). The reaction was allowed to warm to room temperature overnight. The dark red reaction was stirred with potassium carbonate (204 g) for 30 minutes and then filtered and concentrated to dryness. The residue was purified by Biotage, eluting with 3:1 to 2:1 DCM/EtOAc mixture to give the title compound as a white solid (137.0 g, 49% yield).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06800651B2uspto-grants-2004_10