Reaktion #45639

ord-481576c250af446b9a24de058d7cc36c

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled to room temperature
  2. 2
    SonstigeThe aqueous layer was separated
  3. 3
    Extraktionthis was extracted twice with ethyl acetate

Vorschrift

7-Fluoro-2-(2-furyl)-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile (I-105) (40 mg, 0.13 mmol) was dissolved in anhydrous dimethyl sulfoxide (2 ml), and at room temperature, triethylamine (26 μl, 0.19 mmol) and (3S)-3-(dimethylamino)pyrrolidine (21 μl, 0.16 mmol) were added. This mixture liquid was stirred at 90° C. for 11 hours, then cooled to room temperature. This was fractionated with ethyl acetate and saturated brine. The aqueous layer was separated, and this was extracted twice with ethyl acetate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07737166B2uspto-grants-2010_06