Sodium Chloride → 4-Azafluorene

HRID 1093030

反応式

HRID 1093030 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[N:4]=[CH:3][CH:2]=1.O.NN.[Cl-].[Na+]>C(O)COCCO>[CH:1]1[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[N:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 5234Sodium ChlorideHCID 24654Hydrazine hydrate (1:1)HCID 774895H-Indeno(1,2-b)pyridin-5-one

生成物 1

HCID 92054-Azafluorene収率 99%

試薬・触媒・溶媒 1

HCID 8117Diethylene Glycol溶媒

反応条件

温度
168 °C

実験手順

Subsequently, in a stream of argon, 500 mL of diethylene glycol was added to 16.8 g (92.6 mmol) of 4-azafluorene-9-one and 25 mL (370 mmol) of hydrazine monohydrate, and was heated and stirred at 168° C. for 3 hours. After the reaction liquid was cooled to room temperature, an aqueous solution of sodium chloride was added to the reaction liquid, and then, was extracted with ethyl acetate. The organic phase was washed with water, dried over sodium sulfate and concentrated, to thereby obtain 15.3 g of 4-azafluorene (99% yield).

後処理

  1. temperaturewas heated
  2. customAfter the reaction liquid
  3. temperaturewas cooled to room temperature
  4. extractionwas extracted with ethyl acetate
  5. washThe organic phase was washed with water
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-e5ea128c0996488d818612d85c2ddd28
出典データセット
uspto-grants-2012_03
特許番号
US08129899B1

関連ノート

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