Dimethylformamide dimethyl acetal → HCID 67404651, 화합물

HRID 910248노트

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HRID 910248 반응식
CO[CH:3](OC)[N:4]([CH3:6])[CH3:5].[N:9]1[C:10]([C:18]2[CH:23]=[CH:22][C:21]([C:24](=[O:26])[CH3:25])=[CH:20][CH:19]=2)=[CH:11][N:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=12>CN(C)C=O>[CH3:6][N:4]([CH3:5])/[CH:3]=[CH:25]/[C:24]([C:21]1[CH:22]=[CH:23][C:18]([C:10]2[N:9]=[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][N:12]3[CH:11]=2)=[CH:19][CH:20]=1)=[O:26]

참가 물질

4

반응물 2

HCID 78373Dimethylformamide dimethyl acetalHCID 215155611-[4-(Imidazo[1,2-a]pyridin-2-yl)phenyl]ethan-1-one

생성물 1

HCID 67404651HCID 67404651, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
120 °C

실험 절차

Subsequently, N,N-dimethylformamide dimethyl acetal (3.0 mL) was added to a solution of 1-(4-imidazo[1,2-a]pyridin-2-ylphenyl)-1-ethanone (2.13 g) in N,N-dimethylformamide (50 mL), followed by heating at 120° C. for 8 hours. The reaction mixture was cooled to room temperature, and the precipitated solid was recovered through filtration, followed by washing with ethanol. The filtrate was concentrated under reduced pressure. The thus-obtained solid and the residue were subjected to flash chromatography. Fractions eluted by dichloromethane-methanol (30:1) were concentrated under reduced pressure, and the solid was recovered through filtration by use of ethyl acetate. Through the above procedure, (E)-3-dimethylamino-1-(4-imidazo[1,2-a]pyridin-2-ylphenyl)-2-propen-1-one (2.38 g) was yielded.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. filtrationthe precipitated solid was recovered through filtration
  3. washby washing with ethanol
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. washFractions eluted by dichloromethane-methanol (30:1)
  6. concentrationwere concentrated under reduced pressure
  7. filtrationthe solid was recovered through filtration by use of ethyl acetate

출처 및 근거

ORD 기록
ord-3e0c21cf91ca4c4f982c4473d1c8fe1c
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022075B2

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