Reaktion #161383

ord-a146b8ddecdc424cbfd0bb94d34d4a81

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationthis was filtered
  2. 2
    Waschenwashed with water
  3. 3
    SonstigeThe crystals obtained
  4. 4
    Sonstigewere purified by silica gel column chromatography

Vorschrift

To a solution of 2-(2-(3-methoxyphenyl)aminoanilin-5-yl)benzoxazole (see Working Example 31-1) (55.0 mg, 0.166 mmol) in dimethylformamide (2 mL) was added an aqueous solution of acetaldehyde (approx. 90%, 31.2 μL, 0.405 mmol) and oxone (66.3 mg, 0.108 mmol), and this was stirred at room temperature for 3 hours. After the reaction was complete, aqueous potassium carbonate solution was added, this was filtered and washed with water. The crystals obtained were purified by silica gel column chromatography to yield the title compound (17.3 mg, 29% yield) as light brown crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08829035B2uspto-grants-2014_09