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Lansoprazole Intermediate - TFPB Crystal Forms

IP.com Disclosure Number: IPCOM000016611D
Publication Date: 2003-Jul-03
Document File: 4 page(s) / 477K

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Abstract

2-[((3-Methyl-4-(2,2,2-Trifluoroethoxy)-2-Pyridinyl)-Methyl)-Thio]-1H-Benzimidazole (TFPB) is used as intermediate in the preparation of Lansoprazole. Various samples of TFPB were analyzed by X-Ray Powder diffraction and found to contain different crystal forms (I, II, III, IV).

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Lansoprazole intermediate -TFPB Crystal forms

2-[((3-Methyl-4-(2,2,2-Trifluoroethoxy)-2-Pyridinyl)-Methyl)-Thio] -1H-Benzimidazole (TFPB) is used as intermediate in the preparation of Lansoprazole. Various samples of TFPB were analyzed by X-Ray Powder diffraction and found to contain different crystal forms (I, II, III, IV). Form III contains about 14% of Isopropylalcohol and may considered as Isopropylalcohol solvate. Table I summarizes the various samples and suppliers. XRD diffractograms of TFPB form I, II, III and IV are shown in fig. 1-4. Main XRD peaks for the various forms I-IV 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.2J, continuous scan, rate 3 deg/min.

Table I

Sample No. Supplier crystal form Assay

3302300202 Dai-Ichi II 98.1

LSI-602001 Lee Pharma IV

3302300103 Lee Pharma I+II »96%

CN 3302300302

Lee Pharma(LA-3130-1) III 84.9%

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Table II

Crystal form XRD peaks

I 2.9, 5.8, 11.6, 11.8, 12.0, 12.3, 12.5, 13.3, 13.5,

15.1, 18.5, 19.1, 21.7, 22.3, 22.8, 23.2, 23.9, 24.6,

25.6, 26.8, 27.5

II 5.5, 12.6, 15.0, 16.3, 16.6, 18.0, 18.8, 19.8, 20.,

21.3, 25.3

III 5.6, 11.3, 13.2, 15.4, 16.7, 19.0, 20.3, 20.7, 22.7,

22.9, 23.6, 24.0, 24.7, 25.5

IV 5.7, 11.3, 12.7, 14.2, 16.9, 17.5, 18.6, 22.3, 23.4,

24.9, 25.6, 25.8, 27.7

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