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2-Acetylfuran → 4-(Furan-2-yl)-1,3-thiazol-2-amine

HRID 2076915
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HRID 2076915 반응식
[C:1]([C:4]1[O:5][CH:6]=[CH:7][CH:8]=1)(=O)[CH3:2].[Br-].[Br-].[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC.[NH2:63][C:64]([NH2:66])=[S:65]>ClCCl.CO>[NH2:66][C:64]1[S:65][CH:2]=[C:1]([C:4]2[O:5][CH:6]=[CH:7][CH:8]=2)[N:63]=1
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참가 물질

6

반응물 3

HCID 145052-AcetylfuranHCID 2723790ThioureaHCID 23500184Tetra-n-butylammonium tribromide

생성물 1

HCID 7278344-(Furan-2-yl)-1,3-thiazol-2-amine수율 20%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

2-Acetylfuran (5.10 g, 46.0 mmol) was dissolved in a mixed solvent of dichloromethane (50 mL) and methanol (50 mL), and N,N,N,N-tetra-n-butylammonium tribromide (22.3 g, 46.0 mmol) added thereto, then the solution was stirred at room temperature for 1 hour. The reaction mixture was concentrated under reduced pressure, and water was added to the resulting residue, then the mixture was extracted with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate. The solvent was then evaporated under reduced pressure. The resulting residue was dissolved in acetonitrile (60 mL), and thiourea (3.5 g, 46.0 mmol) added thereto, then the solution was stirred at room temperature for 30 minutes. The precipitated solid was collected by filtration, and to the resulting solid was added saturated sodium bicarbonate aqueous solution and ethyl acetate added, then the mixture was extracted. The organic layer was washed with brine and dried over anhydrous magnesium sulfate. The solvent was then evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1) to give 2-amino-4-(2-furyl)thiazole (1.53 g, 20%).

후처리

  1. additionadded
  2. concentrationThe reaction mixture was concentrated under reduced pressure, and water
  3. additionwas added to the resulting residue
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe organic layer was washed with brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe solvent was then evaporated under reduced pressure
  8. dissolutionThe resulting residue was dissolved in acetonitrile (60 mL)
  9. stirringthe solution was stirred at room temperature for 30 minutes
  10. filtrationThe precipitated solid was collected by filtration
  11. additionto the resulting solid was added saturated sodium bicarbonate aqueous solution and ethyl acetate
  12. additionadded
  13. extractionthe mixture was extracted
  14. washThe organic layer was washed with brine
  15. dry with materialdried over anhydrous magnesium sulfate
  16. customThe solvent was then evaporated under reduced pressure
  17. customThe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1)

출처 및 근거

ORD 기록
ord-3c8d6a9e291d4478bc61e89d6e511efb
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07928098B2

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