Sodium Chloride → 4-Azafluorene

HRID 1093030

반응식

HRID 1093030 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[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

참가 물질

5

반응물 3

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

생성물 1

HCID 92054-Azafluorene수율 99%

시약·촉매·용매 1

HCID 8117Diethylene Glycol용매

반응 조건

온도
168 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e5ea128c0996488d818612d85c2ddd28
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08129899B1

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