Water → 5-[2-(Acetylamino)ethylthio]imidazo[1,2-a]pyridine

HRID 1081714노트

반응식

HRID 1081714 반응식
Cl.Cl.[NH2:3][CH2:4][CH2:5][S:6][C:7]1[N:12]2[CH:13]=[CH:14][N:15]=[C:11]2[CH:10]=[CH:9][CH:8]=1.C(N(CC)CC)C.[C:23](Cl)(=[O:25])[CH3:24].O>CN(C)C=O>[C:23]([NH:3][CH2:4][CH2:5][S:6][C:7]1[N:12]2[CH:13]=[CH:14][N:15]=[C:11]2[CH:10]=[CH:9][CH:8]=1)(=[O:25])[CH3:24]

참가 물질

6

반응물 4

HCID 962WaterHCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 233628335-[2-(Amino)ethylthio]imidazo[1,2-a]pyridine dihydrochloride

생성물 1

HCID 233628825-[2-(Acetylamino)ethylthio]imidazo[1,2-a]pyridine수율 66.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 5-[2-(amino)ethylthio]imidazo[1,2-a]pyridine dihydrochloride (2.66 g, 10 mmoles) and triethylamine (4.32 ml, 31 mmoles) in N,N-dimethylformamide (24 ml) was added acetyl chloride (0.71 ml, 10 mmoles) under ice-cooling with stirring and the mixture was stirred at room temperature for 4 hours. The reaction mixture was poured into water and extracted with chloroform. The chloroform layer was washed with saturated saline and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was purified by column chromatography (eluent: ethanol/ethyl acetate=1:3) to obtain 1.57 g of the desired product (66.8%, colorless crystals).

후처리

  1. temperaturecooling
  2. stirringthe mixture was stirred at room temperature for 4 hours
  3. extractionextracted with chloroform
  4. washThe chloroform layer was washed with saturated saline
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationAfter the solvent was distilled off
  7. customthe residue was purified by column chromatography (eluent: ethanol/ethyl acetate=1:3)

출처 및 근거

ORD 기록
ord-0561531abd1b4cafb91701953164856e
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05587383

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