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Acetonitrile → 4-Phenylquinolin-2-amine

HRID 432126
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HRID 432126 반응식
[OH-].[K+].[NH2:3][C:4]1[CH:17]=[CH:16][CH:15]=[CH:14][C:5]=1[C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=O.[C:18](#[N:20])[CH3:19]>>[C:8]1([C:6]2[C:5]3[C:4](=[CH:17][CH:16]=[CH:15][CH:14]=3)[N:3]=[C:18]([NH2:20])[CH:19]=2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 6342Acetonitrile2회HCID 14797Potassium HydroxideHCID 760802-Aminobenzophenone

생성물 1

HCID 6722654-Phenylquinolin-2-amine

실험 절차

Acetonitrile (150 mL) was heated to reflux for 30 minutes in the presence of potassium hydroxide (14.2 g, 254 mmol). 2-amino-benzophenone (10.0 g, 50.7 mmol) in acetonitrile (165 mL) was added to the reaction mixture. After heating to reflux overnight, the mixture was cooled to room temperature, and the resulting solid was filtered. HCl (1.0 M, 100 mL) was added to the solution, and the resulting solid was filtered. The solids were combined, dissolved in ethyl acetate, dried over magnesium sulfate, and filtered. The volatile components were removed with a rotary evaporator, and the solid was recrystallized from ethyl acetate and heptane.

후처리

  1. temperatureAfter heating
  2. temperatureto reflux overnight
  3. filtrationthe resulting solid was filtered
  4. additionHCl (1.0 M, 100 mL) was added to the solution
  5. filtrationthe resulting solid was filtered
  6. dissolutiondissolved in ethyl acetate
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. customThe volatile components were removed with a rotary evaporator
  10. customthe solid was recrystallized from ethyl acetate and heptane

출처 및 근거

ORD 기록
ord-7e52a33688144b61ba511d8fa390bcbb
출처 데이터셋
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06661023B2

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