Hydrochloric Acid → 9-Fluorenone hydrazone

HRID 1241221

반응식

HRID 1241221 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 836279-Fluorenone hydrazone수율 74%

시약·촉매·용매 1

HCID 3776Isopropanol용매

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4e487b3cec564faea8c88468adbf93de
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07115347B2

연결된 노트

불러오는 중…