Reaktion #549115

ord-6f99dc7573184a399922682da6d1ecca

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    Sonstigefor preparing the compounds of the present invention
  2. 2
    workup.ADDITIONIn this examole a mixture containing 12 g
  3. 3
    SonstigeThe mixture is then evaporated under vacuum
  4. 4
    Sonstigeto remove the ethanol solvent
  5. 5
    workup.DISSOLUTIONthe resulting residue dissolved in 50 ml
  6. 6
    Temperaturmaintained at this temperature for two hours
  7. 7
    FiltrationThe mixture is then filtered
  8. 8
    Filtrationthe resulting filter cake
  9. 9
    Waschenwashed with cold (about 0° C) ethyl ether
  10. 10
    Sonstigerecrystallized from ethyl acetate

Vorschrift

This examole illustrates methods for preparing the compounds of the present invention. In this examole a mixture containing 12 g. (0.037 mole) of 1,2-epoxy-3-[5-(hex-5-ynylaminocarbonyl)thiazol-2-yloxy]propane, 12 g. (0.164 mole) of t-butylamine 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 ethanol solvent and the resulting residue dissolved in 50 ml. of ethyl acetate and cooled to -20° C, and maintained at this temperature for two 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-t-butylamino-3-[5-(hex-5-ynylaminocarbonyl)thiazol-2-yloxy]propan-2-ol, m.p. 140°-148° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04064257uspto-grants-1977_12