Cl.Cl.[C:3]([N:6]1[CH2:11][CH2:10][N:9]([NH2:12])[CH2:8][CH2:7]1)(=[O:5])[CH3:4].C(N(CC)CC)C.[S:20]1[CH:24]=[CH:23][CH:22]=[C:21]1[C:25](Cl)=[O:26]>ClCCl.C(OCC)(=O)C>[C:3]([N:6]1[CH2:11][CH2:10][N:9]([NH:12][C:25]([C:21]2[S:20][CH:24]=[CH:23][CH:22]=2)=[O:26])[CH2:8][CH2:7]1)(=[O:5])[CH3:4]To a stirred solution of 1-acetyl-4-aminopiperazine dihydrochloride (250 mg) and triethylamine (0.65 ml) in dichloromethane (9 ml) was added 2-thiophenecarbonyl chloride (0.19 ml) at 0° C. The mixture was stirred at ambient temperature for 1 hour, diluted with ethyl acetate and washed with water (×2). The organic layer was separated, dried over magnesium sulfate, and concentrated. The residue was purified by column chromatography eluting with a mixture of methanol and ethyl acetate (1:10) to give crystals. Recrystallization from ethanol gave N-(4-acetyl-1-piperazinyl)thiophene-2-carboxamide (256 mg).
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