Reaktion #1462255

ord-b4fd66bc22854bfa9c53814ede105903

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigereaction mixture
  2. 2
    Sonstigewas evaporated
  3. 3
    Sonstigeto yield an amber gum
  4. 4
    SonstigeThis gum was triturated with pentane
  5. 5
    Sonstigethe solid obtained
  6. 6
    Waschenwas washed with pentane
  7. 7
    Sonstigedried at 60° C., under vacuum

Vorschrift

[1-{4-[{2-[3-Methoxy-4-[3-o-tolyl-ureido]-phenyl]-acetyl}-methyl-amino]-phenyl}-cyclopentyl]-acetic acid tert-butyl ester [0.18 g, Reference Example 8(b)] was treated with a mixture of trifluoroacetic acid (6 mL), dichloromethane (1.2 mL) and water (0.75 mL)and the resulting solution was then stirred at room temperature, under argon, for 1.5 hours. The amber coloured reaction mixture was evaporated and the residue was chased twice with toluene (20 mL) to yield an amber gum. This gum was triturated with pentane and the solid obtained was washed with pentane and then dried at 60° C., under vacuum, to give the title compound (0.13 g) as a pale yellow solid, m.p. softens at 100° C. then slowly melts from 118–150° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07166616B2uspto-grants-2007_01