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[ R*,S*-(E)]-(±)-7-[3-(4-fluorophenyl)-1-(1-methylethyl)-1 H-indol-2-yl]-3,5-dihydroxy-6-heptenoic acid, monosodium salt intermediate - FDME Crystal forms

IP.com Disclosure Number: IPCOM000018800D
Publication Date: 2003-Aug-11
Document File: 2 page(s) / 141K

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[ R*, S *-( E )]-(±)-7-[3-(4-fluorophenyl)-1-(1-methylethyl)-1 H -indol-2-yl]-3,5-dihydroxy-6-heptenoic acid, monosodium salt intermediate -FDME

Crystal forms

[ R*, S *-( E )]-(±)-7-[3-(4-fluorophenyl)-1-(1-methylethyl)-1 H -indol-2-yl]-3,5- dihydroxy-6-heptenoic acid -methyl ester (FDME) is used as intermediate in the preparation of [ R*, S *-( E )]-(±)-7-[3-(4-fluorophenyl)-1-(1-methylethyl)-1 H -indol-2- yl]-3,5-dihydroxy-6-heptenoic acid, monosodium salt. Different samples of FDME were analyzed by X-Ray Powder diffraction and found to contain different crystal forms (α, β). Table I summarizes the various samples and suppliers. XRD diffractograms of FDME form α, β are shown in fig. 1-2. Main XRD peaks for the various forms α, β are listed in Table II. X-Ray Powder Diffractions were performed on ARL (Scintag) X-Ray powder diffractometer

model X'TRA, Cu-tube, solid state detector. A round standard aluminum sample holder with round zero background quartz plate was used. Scanning parameters: range 2-40 deg.2Θ, continuous scan, rate 3 deg/min.

Table I

Sample No. Supplier Crystal form

1 Cadila α 2 HISUN β

Table II

Crystal form XRD peaks (2θ)

α 9.8, 10.3, 12.0, 13.0, 14.5, 16.1, 17.0, 18.3, 19.0, 19.6, 20.4, 21.3, 22.1,

22.6, 23.2, 23.8, 24.2, 24.8, 25.5, 26.6, 27.3, 28.6, 29.4

β 6.5, 7.9, 9.0, 10.2, 11.7, 12.4, 14.8, 15.5, 17.4, 18.4, 19.2, 20.5, 22.1,

25.4, 29.2

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Fig. 1: XRD diffractogram of FDME form α

              Fig. 2: XRD diffractogram of FDME form...