Reaktion #1847363

ord-7877366897604b82bf401ee7cccf116e

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGThe mixture was stirred at 80° C. for 3 h
  2. 2
    Extraktionthe whole was extracted with methylene chloride
  3. 3
    TrocknenThe organic phase was dried over magnesium sulfate
  4. 4
    Einengenconcentrated under reduced pressure
  5. 5
    Sonstigethe residue was purified by means of HPLC (Merk-Hibar-Lichrospher 100-RP-18, water (0.1% trifluoroacetic acid)/acetonitrile (0.1% trifluoroacetic acid)=80/20→10/90)
  6. 6
    SonstigeThe following was obtained

Vorschrift

7.5 mg of lithium aluminum hydride were initially introduced into 1.5 ml of tetrahydrofuran and the mixture was stirred for 10 min. 6 mg of methyl 5-phenyl-1H-pyrazolo[4,3-c]isoquinoline-3-carboxylate (61) in 1.5 ml of tetrahydrofuran were then added dropwise. The mixture was stirred at 80° C. for 3 h, after which water was added and the whole was extracted with methylene chloride. The organic phase was dried over magnesium sulfate and concentrated under reduced pressure, and the residue was purified by means of HPLC (Merk-Hibar-Lichrospher 100-RP-18, water (0.1% trifluoroacetic acid)/acetonitrile (0.1% trifluoroacetic acid)=80/20→10/90). The following was obtained: 62. C17H13N3O1 (275.31) MS (ESI) 276 (M+H)

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06841556B2uspto-grants-2005_01