Реакция #1328403

ord-4e487b3cec564faea8c88468adbf93de

Уравнение реакции

O=C1c2ccccc2-c2ccccc21
9-Fluorenone
NN.O
hydrazine monohydrate
Cl
hydrochloric acid
NN=C1c2ccccc2-c2ccccc21
9-fluorenone hydrazone
Выход 74.0%

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеequipped with a reflux condenser and a mechanical stirrer
  2. 2
    Температураthe mixture was refluxed for one hour
  3. 3
    Фильтрацияthe crude solid product was harvested by filtration
  4. 4
    ПромывкаThe solid was washed with isopropanol
  5. 5
    Другоеrecrystallized from dioxane

Методика

9-Fluorenone (200 g, 1.1 mol, from Aldrich, Milwaukee, Wis.) and hydrazine monohydrate (160 ml, 3.3 mol, from Aldrich, Milwaukee, Wis.) were dissolved in 1000 ml of 2-propanol in a 2000 ml 2-neck round bottom flask equipped with a reflux condenser and a mechanical stirrer. Concentrated hydrochloric acid (4 ml) was then added, and the mixture was refluxed for one hour. The mixture was cooled slowly to room temperature, and the crude solid product was harvested by filtration. The solid was washed with isopropanol and then recrystallized from dioxane to obtain 150 g (74% yield) of 9-fluorenone hydrazone.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07115347B2uspto-grants-2006_10