반응 #1328403

ord-4e487b3cec564faea8c88468adbf93de

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타equipped with a reflux condenser and a mechanical stirrer
  2. 2
    온도the mixture was refluxed for one hour
  3. 3
    여과the crude solid product was harvested by filtration
  4. 4
    세척The solid was washed with isopropanol
  5. 5
    기타recrystallized from dioxane

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07115347B2uspto-grants-2006_10