Reaktion #1931685

ord-4e1a3b5185124e079c66a717fc1b1ff5

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe mixture was reacted at 100° C. for 4 hours
  2. 2
    SonstigeAfter completion of the reaction
  3. 3
    Sonstigeresulting in a substantial amount of precipitate
  4. 4
    FiltrationThen, the precipitate was suction-filtered
  5. 5
    Sonstigethe filter cake was recrystallized with acetone

Vorschrift

Compound 17a (1 g, 6.9 mmol) obtained from the aforesaid process and 3,4-difluoro-nitrobenzene (0.74 mL) were dissolved in N,N-dimethylformamide (20 mL), and then anhydrous potassium carbonate (1.9 g) was added thereto. The mixture was reacted at 100° C. for 4 hours. After completion of the reaction, the reactant mixture was cooled to room temperature. Water was added to the mixture, resulting in a substantial amount of precipitate. Then, the precipitate was suction-filtered, and the filter cake was recrystallized with acetone to get the product 18a as a white powder (1.7 g), with a yield of 93.4%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08946436B2uspto-grants-2015_02