Hydrochloric Acid → HCID 17955463, compound

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A mixture of 3-{[2-(9H-fluoren-9-yl)-ethyl]-methyl-amino}-propionic acid chloride hydrochloride (1.14 g), 4-(3,4-Difluoro-phenyl)-piperazine (587 mg), dichloromethane (25 ml) and 1 M aq. K2CO3 (25 ml) is stirred at room temperature for 1 hour. The phases are separated, the organic phase dried over sodium sulfate, filtered and evaporated. Purification by chromatography on silicagel (EtOAc/MeOH 7:3) afforded 1.2 g (100%) of a slightly colored oil. It is dissolved in 4 ml MeOH and acidified with 6 ml 1 M HCl in diethyl ether. More ether is added until the solution gets cloudy (ca. 3 ml). Crystallization at 5° afford 1.01 g (74%) of the desired product as dihydrochloride. M.p. 144°-154°. Anal: Calculated. for C29H33Cl2F2N3O.H2O: C, 61.48%; H, 6.22%; N, 7.41%. Found: C, 61.52%; H, 6.36%; N, 7.37%.

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