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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ethanol → 2-Fluoro-4'-aminobenzophenone

HRID 865254
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HRID 865254 반응식
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=O.[NH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(O)C>O>[NH2:11][C:12]1[CH:17]=[CH:16][C:15]([C:4]([C:3]2[CH:7]=[CH:8][CH:9]=[CH:10][C:2]=2[F:1])=[O:6])=[CH:14][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 6115AnilineHCID 99352-Fluorobenzoic acid

생성물 1

HCID 105128532-Fluoro-4'-aminobenzophenone수율 253.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To stirred 90° C. polyphosphoric acid (200 g) was added 14.29 g (10.2 mmol) of 2-fluorobenzoic acid and aniline (9.32 g 10.0 mmol) and the bath temperature raised to 180°-190° C. and held there for 1 hour. A solution was obtained at about 140° C. The heating bath was removed and the stirred mixture (sublimate above the solution) was treated cautiously with 80 mL of water. The mixture was stirred at 140°-155° C. for 1 hour, the heating bath removed, 66 mL of 3N HCl added, the mixture poured into 1L of water and filtered through a pad of Celite. The liltrate was basilled with 15% sodium hydroxide and the solid which formed on stirring was collected. The Celite pad was washed well with methylene chloride, the methylene chloride removed and the residue was combined with the solid obtained from basification of the aqueous phase. The combined material was dissolved in refluxing ethanol (175 mL), and treated hot with 125 mL of water. The brown solid obtaing on cooling was additionally recrystallized twice from ethyl acetate - hexane. Final purification by flash column chromatography (methylene chloride) yielded the aniline as a white solid (5.45 g, 25%); mp 128°-130° C. 1H-NMR (250 MHz, d6-DMSO): 6.32 (s, 2H, NH2) 6.60 (dd, 2H, J=8.6, 1.5 Hz, aromatic) 7.28-7.35 (m, 2H, aromatic) 7.40-7.60 (m, 4H, aromatic). MS (CI, CH4): 216 (M+1).

후처리

  1. temperaturethe bath temperature raised to 180°-190° C.
  2. customA solution was obtained at about 140° C
  3. customThe heating bath was removed
  4. additionthe stirred mixture (sublimate above the solution) was treated cautiously with 80 mL of water
  5. customthe heating bath removed
  6. addition66 mL of 3N HCl added
  7. additionthe mixture poured into 1L of water
  8. filtrationfiltered through a pad of Celite
  9. customthe solid which formed
  10. stirringon stirring
  11. customwas collected
  12. washThe Celite pad was washed well with methylene chloride
  13. customthe methylene chloride removed
  14. customobtained from basification of the aqueous phase
  15. dissolutionThe combined material was dissolved
  16. temperatureThe brown solid obtaing on cooling
  17. customwas additionally recrystallized twice from ethyl acetate - hexane
  18. customFinal purification by flash column chromatography (methylene chloride)

출처 및 근거

ORD 기록
ord-7dc29f96500647ec802d9cc4d3c408b8
출처 데이터셋
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05565477

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