Reaktion #708737

ord-991eddb2af6c4c9aad9ac27f672eeaa6

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigereacted at 50°-60° C. for 3 hours
  2. 2
    Einengenthe reaction mixture is concentrated under a reduced pressure
  3. 3
    SonstigeTo the residue thus obtained
  4. 4
    workup.DISSOLUTIONto dissolve the residue uniformly
  5. 5
    SonstigeThe crystals precipitated
  6. 6
    Filtrationare collected by filtration
  7. 7
    Sonstigedried
  8. 8
    SonstigeRecrystallization from water

Vorschrift

4.4 grams of 5-(2,3-epoxypropoxy)-3,4-dihydrocarbostyril and 3.4 g of 4-phenylpiperazine are dispersed in 60 ml of methanol and reacted at 50°-60° C. for 3 hours. After the reaction is completed, the reaction mixture is concentrated under a reduced pressure. To the residue thus obtained are added 5 ml of concentrated hydrochloric acid and 30 ml of ethanol to dissolve the residue uniformly and further 200 ml of acetone are added. The crystals precipitated are collected by filtration and dried. Recrystallization from water to obtain 6.5 g of 5-[2-hydroxy-3-(4-phenylpiperazinyl)propoxy]-3,4-dihydro carbostyril monohydrochloride in the form of colorless needle-like crystals with a melting point of 239°-241° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04824840uspto-grants-1989_04