Diisopropylethylamine → (S)-N4-[(S)-1-(amino-imino-methyl)-piperidin-3-ylmethyl]-N1-cyclopropyl-N1-[2-(4-methyl-piperazin-1-ylsulphonylamino)-ethyl]-2-morpholin-4-ylsulphonylamino-succinamide acetate

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Reaction Steps

330 mg of (S)-N1-(2-amino-ethyl)-N4-[(S)-1-(amino-imino-methyl)-piperidin-3-ylmethyl]-N1-cyclopropyl-2-morpholin-4-ylsulphonylamino-succinamide hydrochloride are stirred at room temperature for 20 hours together with 162 mg of 4-methyl-piperazin-1-ylsulphonyl chloride and 0.49 ml of Hunig's base in 8 ml of methylene chloride. The reaction mixture is chromatographed over silica gel with ethyl acetate/acetone/glacial acetic acid/water 2:2:2:1. 14.9.1 mg of pure crystalline (S)-N4-[(S)-1-(amino-imino-methyl)-piperidin-3-ylmethyl]-N1-cyclopropyl-N1-[2-(4-methyl-piperazin-1-ylsulphonylamino)-ethyl]-2-morpholin-4-ylsulphonylamino-succinamide acetate (1:2), MS (ISP): 665.6 (M+H) and 333.7 (M+2H), are obtained.

Provenance & Evidence