Reaktion #548871

ord-631af8bf49954f2f8bc620956a80e367

Lösungsmittel

Reaktionsbedingungen

Temperatur
-20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigefor preparing the compounds of formula C
  2. 2
    SonstigeThe mixture is then evaporated under vacuum
  3. 3
    Sonstigeto remove the solvent
  4. 4
    workup.DISSOLUTIONthe resulting residue dissolved in 50 ml
  5. 5
    Temperaturmaintained at this temperature for 2 hours
  6. 6
    FiltrationThe mixture is then filtered
  7. 7
    Filtrationthe resulting filter cake
  8. 8
    Waschenwashed with cold (about 0° C) ethyl ether
  9. 9
    Sonstigerecrystallized from ethyl acetate

Vorschrift

This example illustrates processes of the invention for preparing the compounds of formula C. In this example a mixture containing 12 g. (0.0314 mole) of 1,2-epoxy-3-(5-[2-(adamant-2-yl)ethylaminocarbonyl]thiazol-2-yloxy)propane, 12 g. (0.203 mole) of isopropylamine and 20 ml. of ethanol is allowed to stand at room temperature for 12 hours. The mixture is then evaporated under vacuum to remove the solvent and the resulting residue dissolved in 50 ml. of ethyl acetate and cooled to -20° C, and maintained at this temperature for 2 hours. The mixture is then filtered and the resulting filter cake washed with cold (about 0° C) ethyl ether and then recrystallized from ethyl acetate affording 1-isopropylamino-3-(5-[2-(adamant-2-yl)ethylaminocarbonyl]thiazol-2-yloxy)-propan-2-ol.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04064135uspto-grants-1977_12