تفاعل #1328403

ord-4e487b3cec564faea8c88468adbf93de

معادلة التفاعل

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

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىequipped with a reflux condenser and a mechanical stirrer
  2. 2
    درجة الحرارةthe mixture was refluxed for one hour
  3. 3
    ترشيحthe crude solid product was harvested by filtration
  4. 4
    غسيلThe solid was washed with isopropanol
  5. 5
    أخرىrecrystallized from dioxane

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07115347B2uspto-grants-2006_10