반응 #816017

ord-757f059b791243d6aa07ddc3f7e17afc

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타remove the solvents in vacuo
  2. 2
    workup.DISSOLUTIONDissolve the residue in glacial acetic acid with 0.86 g10% palladium hydroxide on carbon
  3. 3
    기타the progress of the reaction by thin-layer chromatography on silica gel (acetonitrile:ammonia,9:1)
  4. 4
    기타At the completion of the reaction
  5. 5
    여과the catalyst is filtered
  6. 6
    기타the solvents are removed in vacuo
  7. 7
    기타The resulting oil is chromatographed on alumina (activity III)

실험 절차

Dissolve 6.36 g (.013 mol) 1-[[2-[4-(1H-imidazol-1-yl)phenoxy]ethyl](phenylmethyl)amino]-3-[4-(2-methoxyethyl)phenoxy]-2-propanol in 50 mL 5 M methanolic HCl and remove the solvents in vacuo. Dissolve the residue in glacial acetic acid with 0.86 g10% palladium hydroxide on carbon. The reaction mixture is hydrogenated under 52 psi H2 on a Parr Hydrogenator. Follow the progress of the reaction by thin-layer chromatography on silica gel (acetonitrile:ammonia,9:1). At the completion of the reaction, the catalyst is filtered and the solvents are removed in vacuo. The resulting oil is chromatographed on alumina (activity III) using 2% methanol in methylene chloride to provide the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05051423uspto-grants-1991_09