Hydrochloric Acid → 9-Fluorenone hydrazone

HRID 1241221

反応式

HRID 1241221 の反応式
[CH:1]1[C:13]2[C:12](=O)[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.O.[NH2:16][NH2:17].Cl>CC(O)C>[CH:1]1[C:13]2[C:12](=[N:16][NH2:17])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 10241FluorenoneHCID 24654Hydrazine hydrate (1:1)

生成物 1

HCID 836279-Fluorenone hydrazone収率 74%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  1. customequipped with a reflux condenser and a mechanical stirrer
  2. temperaturethe mixture was refluxed for one hour
  3. filtrationthe crude solid product was harvested by filtration
  4. washThe solid was washed with isopropanol
  5. customrecrystallized from dioxane

出典と根拠

ORDレコード
ord-4e487b3cec564faea8c88468adbf93de
出典データセット
uspto-grants-2006_10
特許番号
US07115347B2

関連ノート

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