Reaktion #337667

ord-ac7adb84eb90486bbfa19d3b1c71930c

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe resulting mixture was reacted in the microwave at 100° C. for 10 min
  2. 2
    Filtrationthe resulting precipitate was filtered
  3. 3
    Waschenwashed with water
  4. 4
    Sonstigedried
  5. 5
    SonstigeFurther purification by silica gel chromatography

Vorschrift

To an 80 mL microwave reaction vessel was added (5-nitro-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-acetic acid ethyl ester (2 g), 3,5-difluorophenol (1.12 g), potassium carbonate (1.39 g), and dimethyl acetamide (27 mL). The resulting mixture was reacted in the microwave at 100° C. for 10 min. Water (280 mL) was added and the resulting precipitate was filtered, washed with water and dried. Further purification by silica gel chromatography generated 0.94 g of the title compound. 1H NMR (200 MHz, CDCl3) δ 7.86 (d, J=8.2 Hz, 1H), 7.41-7.31 (m, 2H), 6.67-6.57 (m, 3H), 4.41 (s, 2H), 4.22 (q, J=7.1 Hz, 2H), 1.29 (t, J=7.0 Hz, 3H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07863292B2uspto-grants-2011_01