Reaktion #1924574

ord-efd9c390287548859a18f29cf5d1b609

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe resulting mixture was reacted at 150° C. for 5 hours
  2. 2
    Waschenwashed with 5% hydrochloric acid several times
  3. 3
    ExtraktionThe combined organic extract
  4. 4
    Waschenwas washed with water several times
  5. 5
    Trocknendried with anhydrous magnesium sulfate
  6. 6
    SonstigeThe solvent was removed
  7. 7
    Sonstigeto obtain solid, which
  8. 8
    Sonstigewas recrystallized from ethyl acetate

Vorschrift

Under an argon atmosphere, 15 g (74 mmol) of 1,4-di-phenylbutadiyne, 12.76 g (74 mmol) of p-bromoaniline and 1.84 g (18 mmol) copper(I) chloride were put into 500 ml round-bottomed flask, and the resulting mixture was reacted at 150° C. for 5 hours while stirring. After the reaction was completed, the reaction mixture was cooled down to room temperature, dissolved in chloroform and then washed with 5% hydrochloric acid several times. The combined organic extract was washed with water several times and then dried with anhydrous magnesium sulfate. The solvent was removed to obtain solid, which was recrystallized from ethyl acetate to give 20.4 g (73.5%) white solid having a melting point of 218-219° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06780950B2uspto-grants-2004_08