Hydrazine hydrate (1:1) → 4-Azafluorene

HRID 578603

반응식

HRID 578603 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]2[C:7](=O)[C:8]3[C:13]([C:2]=12)=[CH:12][CH:11]=[CH:10][CH:9]=3.O.NN>C(O)COCCO>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]2[CH2:7][C:8]3[C:13]([C:2]=12)=[CH:12][CH:11]=[CH:10][CH:9]=3

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 774895H-Indeno(1,2-b)pyridin-5-one

생성물 1

HCID 92054-Azafluorene수율 81%

시약·촉매·용매 1

HCID 8117Diethylene Glycol용매

반응 조건

온도
170 °C

실험 절차

A mixture of 18.1 g (100 mmol) of 5H-indeno[1,2-b]pyridin-5-one, 27 ml (400 mmol) of hydrazine monohydrate, and 500 ml diethylene glycol was degassed and placed under nitrogen, and then heated at 170° C. for 12 h. After the reaction finish, the mixture was allowed to cool to room temperature. The organic layer was extracted with ethyl acetate and water, dried with anhydrous magnesium sulfate, the solvent was removed to give product 13.5 g (81%).

후처리

  1. customwas degassed
  2. temperatureto cool to room temperature
  3. extractionThe organic layer was extracted with ethyl acetate and water
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customthe solvent was removed

출처 및 근거

ORD 기록
ord-9485400a145141718cd19b05d8275b9d
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040174B2

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