Y. Osa, Yoko Sato, A. Hatano
Sep 1, 2002
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Analytical Sciences
Abstract
5-yl)piperazine (1) (Fig. 1) are useful compounds because of their high biological activity, especially their multidrug resistance (MDR) in cancer.1,2 We also found that the derivatives of 1 have a recovering activity for MDR in malaria. However, as a basic compound, the crystal and molecular structure of 1 has not been clearly established. The title compound 1 was obtained by the reaction of dibenzosuberyl chloride with piperazine in toluene under the presence of 1,8diazabicyclo[5.4.0]undec-7-ene (DBU) in 78% yield as a hydrochloride salt giving a higher melting point than those of the previous reports.1,2 The solid was crystallized from CHCl3AcOEt. The chemical shifts of 1H-NMR (600 MHz) spectrum supported the chemical structure of hydrochloride of 1. It was found that the chemical shifts of the salt were slightly observed in a lower field compared with those of the free form. In this paper, we present the crystal structure of hydrochloride of 1. Single crystals for X-ray structure were obtained from MeOH/H2O by slow evaporation. The crystal and experimental data are given in Table 1. The structure was solved by a direct method with SIR-92.3 Hydrogen atoms of piperazine were located from the difference Fourier map and refined isotropically, but other hydrogens were 1069 ANALYTICAL SCIENCES SEPTEMBER 2002, VOL. 18 2002 © The Japan Society for Analytical Chemistry