반응 #719050

ord-ccad89960a8445c1984729ffe298fdba

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated
  2. 2
    온도at reflux for 72 hours
  3. 3
    여과The reaction mixture was filtered through celite
  4. 4
    기타the filtrate was evaporated under vacuum
  5. 5
    기타The residue was purified by flash chromatography on silica
  6. 6
    세척eluting with a mixture of DCM and methanol
  7. 7
    workup.ADDITIONThe fractions containing the desired product
  8. 8
    기타evaporated

실험 절차

A mixture of N-[2-(1-benzyl-1H-tetrazol-5-yl)-3-methoxyphenyl]-benzenesulfonamide (Intermediate 12, 0.104 g), ammonium formate (0.45 g) and palladium hydroxide (0.01 g) in ethanol (10 mL) was heated at reflux for 72 hours. The reaction mixture was filtered through celite and the filtrate was evaporated under vacuum. The residue was purified by flash chromatography on silica, eluting with a mixture of DCM and methanol. The fractions containing the desired product were combined and evaporated to give the title compound as a colorless solid (0.05 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09321740B2uspto-grants-2016_04