Reaktion #1836142

ord-5a01094a2a69470cb3aab8f5adde4919

Lösungsmittel

Reaktionsbedingungen

Temperatur
130°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeIn a 300 mL recovery flask were put
  2. 2
    workup.DISTILLATIONAfter that, 1-butanol was distilled off
  3. 3
    Sonstigeto give a solid
  4. 4
    Sonstigewas irradiated with ultrasonic waves
  5. 5
    Filtrationa white solid was collected by gravity filtration, so that 2.8 g of white powder of 4-(4-bromophenyl)-5-isopropyl-3-phenyl-4H-1,2,4-triazole
  6. 6
    Sonstigewas obtained in a yield of 28%
  7. 7
    SonstigeThe reaction scheme of Step 4

Vorschrift

In a 300 mL recovery flask were put 13 g (44 mmol) of N-[1-(ethylsulfanyl)isobutylidene]-4-bromoaniline, 3.9 g (29 mmol) of benzoylhydrazine, and 40 mL of 1-butanol, and the mixture was heated and refluxed at 130° C. for 10 hours. After that, 1-butanol was distilled off to give a solid. A methanol suspension of this solid was irradiated with ultrasonic waves, and a white solid was collected by gravity filtration, so that 2.8 g of white powder of 4-(4-bromophenyl)-5-isopropyl-3-phenyl-4H-1,2,4-triazole was obtained in a yield of 28%. The reaction scheme of Step 4 is shown in (b-4) below.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09155158B2uspto-grants-2015_10