Reaktion #558648

ord-4f8f9a9edec64f1abf3b4b0c887b8a32

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe precipitation
  2. 2
    Filtrationwas collected by filtration
  3. 3
    Waschenwashed with EtOAc/Hexanes (1:4)
  4. 4
    Sonstigedried under vacuum overnight

Vorschrift

To a solution of 2-amino-4,5-dimethylthiophene-3-carbonitrile (1.52 g, 10.0 mmol) in 1,4-dioxane (20 mL) was added benzoylisothiocyanate (1.63 g, 10.0 mmol). The reaction mixture was then stirred at room temperature under nitrogen overnight. The precipitation was collected by filtration, washed with EtOAc/Hexanes (1:4), and dried under vacuum overnight to give N-(3-Cyano-4,5-dimethylthiophen-2-ylcarbamothioyl)benzamide as a white solid. 1H NMR (400 MHz, CDCl3) δ 2.23 (s, 3H), 2.31 (s, 3H), 7.58-7.54 (m, 2H), 7.68-7.66 (m, 1H), 7.94 (d, J=7.2 Hz, 2H), 9.13 (bs, 1H). MS 316 (MH+).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08633186B2uspto-grants-2014_01