Reaktion #44518

ord-6c9f9b57843d4fe9a20c843dfd7e6fce

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionsubjected to extraction with ethyl acetate
  2. 2
    workup.ADDITIONThen water was added
  3. 3
    Extraktionthe mixture was subjected to extraction with ethyl acetate
  4. 4
    WaschenThe organic layer was washed with water and brine sequentially
  5. 5
    Trocknendried over anhydrous Na2SO4
  6. 6
    Einengenconcentrated
  7. 7
    SonstigeThe resulting residue was purified by column chromatography

Vorschrift

6-(2-chloropyrimidin-4-yloxy)-N,2-dimethylbenzofuran-3-carboxamide (0.1 mmol) and 3-methoxyaniline (0.1 mmol) were dissolved in 0.5 ml DMF. To this was added p-TsOH monohydrate (0.2 mmol). The reaction mixture was stirred at 60° C. for 5 hours, and subjected to extraction with ethyl acetate. Then water was added and the mixture was subjected to extraction with ethyl acetate. The organic layer was washed with water and brine sequentially, dried over anhydrous Na2SO4, and concentrated. The resulting residue was purified by column chromatography to provide the title product in a yield of 80%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07737157B2uspto-grants-2010_06