Reaktionsgleichung
[NH2:1][CH2:2][CH2:3][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.Cl[C:24]([O:26][CH:27]([CH3:29])[CH3:28])=[O:25]>C(Cl)Cl>[CH:27]([O:26][C:24]([NH:1][CH2:2][CH2:3][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])([CH3:29])[CH3:28]Komponenten
5
Versuchsvorschrift
To a solution of 5-[4-(amino)butylthio]imidazo[1,2-a]pyridine (370 mg, 1.67 mmoles) and triethylamine (0.35 ml, 2.51 mmoles) in metylene chloride (20 ml) was added isopropyl chloroformate (0.25 g, 2.04 mmoles) under ice-cooling with stirring and the mixture was stirred under ice-cooling for 1 hour. The reaction mixture was washed in turn with an aqueous sodium bicarbonate solution and saturated saline and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was purified by column chromatography (eluent: ethyl acetate) to obtain 215 mg of the desired product (41.8%, light tan oily product).
Aufarbeitung
- temperaturecooling
- stirringthe mixture was stirred under ice-
- temperaturecooling for 1 hour
- washThe reaction mixture was washed in turn with an aqueous sodium bicarbonate solution and saturated saline
- dry with materialdried over anhydrous magnesium sulfate
- distillationAfter the solvent was distilled off
- customthe residue was purified by column chromatography (eluent: ethyl acetate)
Quellen und Nachweise
- ORD-Eintrag
- ord-ce3b6cc6c0d44d898ee55cbe4e28ea20
- Quelldatensatz
- uspto-grants-1993_09
- Patentnummer
- US05244908
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