Réaction #2139931

ord-cae24a0eeab24a9fa894fc57cc059d38

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autreequipped with a mechanical stirrer and an addition funnel
  2. 2
    workup.STIRRINGthe reaction mixture was stirred at room temperature for 2 hours
  3. 3
    FiltrationA precipitate was collected by filtration
  4. 4
    Lavagewashed repeatedly with water
  5. 5
    Autreto give crude, i.e.
  6. 6
    Autrewithout further purification, 9-ethyl-3-carbazolecarboxaldehyde hydrazone, which

Mode opératoire

A quantity of 98% hydrazine monohydrate (50 ml, 1.4 mole, obtained from Aldrich, Milwaukee, Wis.) and 10 ml of triethylamine (obtained from Aldrich, Milwaukee, Wis.) were added to a 250 ml, 2-neck round bottom flask equipped with a mechanical stirrer and an addition funnel. The solution was stirred vigorously at room temperature for a period of 10-15 min. A solution of 9-ethyl-3-carbazolecarboxaldehyde (22.3 g, 0.1 mol, from Aldrich, Milwaukee, Wis.) in 30 ml of tetrahydrofuran (THF) was added slowly to the round bottom flask. After the addition of aldehyde was completed, the reaction mixture was stirred at room temperature for 2 hours. Then, the reaction mixture was diluted with 50 ml of water. A precipitate was collected by filtration and washed repeatedly with water to give crude, i.e. without further purification, 9-ethyl-3-carbazolecarboxaldehyde hydrazone, which was used immediately in the next step.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07326506B2uspto-grants-2008_02