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

HRID 5443

反応式

HRID 5443 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-c70f3f1b3dc840cb9734132ec78a68c7
出典データセット
uspto-grants-1993_09
特許番号
US05244908

関連ノート

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