Reaktion #2066957

ord-5efdf3e0154d4c9eb72d29f9c0f4f1e9

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction mixture was concentrated under a reduced pressure and to the residue
  2. 2
    Sonstigethus obtained
  3. 3
    workup.STIRRINGstirred
  4. 4
    SonstigeThe precipitates thus
  5. 5
    Sonstigeformed
  6. 6
    Filtrationwere collected by filtration
  7. 7
    Waschenwashed with acetone
  8. 8
    Sonstigerecrystallized from methanol-ethanol

Vorschrift

2.0 Grams of 5-[2-hydroxy-3-(4-phenyl-1-piperidyl)propoxy]-3,4-dihydrocarbostyril and 3 g of methyl iodide were mixed with 30 ml of dimethylformamide and the mixture was stirred at 50°-60° C. for 5 hours. The reaction mixture was concentrated under a reduced pressure and to the residue thus obtained was added 50 ml of acetone and stirred. The precipitates thus formed were collected by filtration and washed with acetone, then recrystallized from methanol-ethanol to obtain 1.7 g of 4-phenyl-1-[2-hydroxy-3-(2-oxo-1,2,3,4-tetrahydroquinolin-5-yloxy)propyl]-1-methylpiperidiniumiodide as in the form of colorless powdery substance. Melting point: 242°-243° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04482560uspto-grants-1984_11