alpha-Selective epoxidation of 3 beta-chlorocholest-5-ene and 3 beta-acetoxycholest-5-ene has been performed with m-CPBA to synthesize 3 beta-chloro-5 alpha,6 alpha-epoxycholestane (1) and 3 beta-acetoxy-5 alpha,6 alpha-epoxycholesLane (2). We provided an analysis of these compounds by means of FT-IR, FT Raman, H-1 NMR, C-13 NMR, 20 cosy, NOESY. UV -visible and X-ray crystallography. The compound 1 crystallizes in the orthorhombic space group P2(1)2(1)2(1) while compound 2 crystallizes in the monoclinic space group P2(1). We compared the conformations of both compounds in solid state and in solution by calculation of dihedral angles and coupling constant values. The povvcler X-ray diffraction (PXRD) of the compound was recorded to ascertain the purity of the grown crystals. Thermogravimetric analysis showed stability of the compounds up to 250 degrees C. Moreover, the ICH rule has been applied to Lest the stability of two crystals, vvhich shovvecl significant stability. (C) 2013 Elsevier B.V. All rights reserved.