Hydrazine hydrate (1:1) → 4-Azafluorene

HRID 578603

反応式

HRID 578603 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 92054-Azafluorene収率 81%

試薬・触媒・溶媒 1

HCID 8117Diethylene Glycol溶媒

反応条件

温度
170 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-9485400a145141718cd19b05d8275b9d
出典データセット
uspto-grants-2015_05
特許番号
US09040174B2

関連ノート

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