Methanesulfonic Acid → 1-[N-cyclohexylcarbonyl-N-(2-pyridyl)-2-aminoethyl]-4-(2,5-dichlorobenzyl)pipe-razine methanesulfonate hemihydrate

Beteiligte Stoffe

Reaktionsschritte

To a mixture comprising 0.164 g of Compound 1B of Example 1, 0.210 g of Compound 14B, and 4 mL methanol, continuously stirred under nitrogen, at room temperature, there was added 0.049 g of sodium cyanoborohydride. The resulting mixture was then stirred for 13 hr, at room temperature, followed by dilution with 10 mL water, and subsequent extraction with ethyl acetate (3×10 mL). The collected organic phases were then dried over anhydrous sodium sulphate, followed by vacuum evaporation, and subsequent purification of the obtained product residue by flash chromatography (chloroform—methanol 95:5). The solvents were then evaporated off, from the recovered fractions, yielding a residual substance which was then solubilized into 2 mL ethyl acetate. To this solution was then added 0.08 mL methanesulphonic acid (2 M solution of CH3SO3H, in ethanol) followed by diethyl ether, until the complete precipitation of the product. 0.071 g of this end-product precipitate was recovered here (yield 19%), through the use of vacuum filtration procedures.

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