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Crystallization methods for 2-chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride

A technology for crude methoxypyridine hydrochloride and methoxypyridine hydrochloride, which is applied in the field of synthesis of pharmaceutical intermediates, can solve the problems of qualitative change in post-treatment, instability of omeprazole, etc., and achieve stable yield and method Simple and convenient effect

Inactive Publication Date: 2014-07-09
ANHUI COSTAR BIOCHEM CO LTD
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  • Description
  • Claims
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Problems solved by technology

The three crystal forms are obtained by different post-treatment methods, and due to the instability of omeprazole, too much post-treatment is prone to qualitative change

Method used

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  • Crystallization methods for 2-chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride
  • Crystallization methods for 2-chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride
  • Crystallization methods for 2-chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride

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Embodiment Construction

[0013] Take 1.00 g of 2-chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride, dissolve it completely with 15 mL of an equal volume mixture of ethanol and acetone, filter out impurities, and place it in a specific room After slow evaporation, 0.43 g of single crystal 2-chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride was obtained after 48 h, with a yield of 43%. The crystalline crystals are monoclinic with space group P 2 1 / c , the unit cell parameters of the crystal: a = 6.074(11), b = 19.88(4), c = 9.230(16) ?, = 99.67(4) , V = 1098(3) ? 3 , Z = 4, M r = 221.10, D c = 1.343 g / cm 3 , (Mo K ) = 0.553 mm , F (000) = 464, S = 0.988. single molecule through hydrogen bonds to form a dimeric structure, such as figure 1 , figure 2 is the unit cell packing diagram formed by dimerized molecules.

[0014] Table 1

[0015]

[0016] Take 1.00 g of 2-chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride, dissolve it complet...

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Abstract

The invention discloses crystallization methods for 2-chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride, which belongs to the technical field of synthesis of drug intermediates. A monocrystalline crystallization method comprises the following steps: dissolving a crude 2-chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride product with a mixed solution of ethanol and acetone and then carrying out dilution; and carrying out filtering so as to remove impurities, placing an obtained filtrate in room temperature and carrying out slow volatilization and crystallization for 48 h so as to obtain monocrystalline 2-chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride. A polycrystalline crystallization method comprises the following steps: subjecting the crude 2-chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride product to heating reflux with a mixed solution of ethanol and acetone until the crude product is completely dissolved; and carrying out filtering as the dissolved crude product is still hot so as to remove impurities and then carrying out slow cooling so as to obtain polycrystalline 2-chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride. The methods provided by the invention are simple and convenient, enable yield to be stable and facilitate development and preparation of high-purity monocrystalline / polycrystalline omeprazole.

Description

field of invention [0001] The invention belongs to the technical field of synthesis of pharmaceutical intermediates, and in particular relates to a crystallization treatment method for 2-chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride. Background technique [0002] Chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride is an important intermediate in the synthesis of omeprazole and esomeprazole. So far, omeprazole has been found to have three Seed crystal forms: Type A, Type B and Type C. Type B omeprazole was first described by Ohishi H et al. The preparation method and characterization data of Type B omeprazole were compared in detail with the differences between Type B and Type B; followed by Patent WO 2002 / 085889, Type C Omeprazole was discovered, and its preparation method was compared with Type A and Type B. Form B is simpler and has a higher yield. The three crystal forms were obtained by different post-treatment methods, and due to the instability of o...

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Application Information

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IPC IPC(8): C07D213/68C07D401/12
CPCC07D213/68
Inventor 刘善和张千峰范芳芳夏佳美
Owner ANHUI COSTAR BIOCHEM CO LTD
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