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Preparation method of mometasone furoate monohydrate

A kind of technology of mometasone furoate and monohydrate, applied in a new preparation field

Active Publication Date: 2013-07-31
TIANJIN JINYAO GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Initially flunisolide hemihydrate was prepared by chlorofluorocarbons (see US4273710), but chlorofluorocarbons are more toxic and often lead to unqualified solvent residues. Later, by looking for other suitable solvents, using carbon chains in 3 or 4 The ol post properly solves the problem

Method used

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  • Preparation method of mometasone furoate monohydrate
  • Preparation method of mometasone furoate monohydrate
  • Preparation method of mometasone furoate monohydrate

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Dissolve 1 g of mometasone furoate in 8 mL of DMF at 55°C, add 35 mL of water, then drop to room temperature (25°C) at a rate of 0.1°C / min; 0.93 g of mometasone furoate hydrate crystals are precipitated. Tested by the Karl Fischer method, the moisture content is 3.32%

[0028] And the obtained crystal is subjected to X-ray powder diffraction measurement, and the measured characteristic peak positions are 2θ=7.8, 11.5, 12.8, 14.1, 15.1, 15.6, 16.6, 17.5, 18.6, 20.1, 21.9, 23.2, such as figure 1 shown.

Embodiment 2

[0030] Dissolve 1 g of mometasone furoate in 8 mL of THF at 45°C, add 20 mL of water, and then evaporate at 60°C for 3 hours; 0.92 g of mometasone furoate hydrate crystals are precipitated. Tested by the Karl Fischer method, the moisture content is 3.41%

Embodiment 3

[0032] Add 1g of mometasone furoate to 10mL of DMSO, heat to reflux, dissolve, slowly add 15mL of water, and then drop to room temperature (25°C) at a rate of 0.1°C / min; 0.91% crystallization of mometasone furoate hydrate is precipitated g. Tested by the Karl Fischer method, the moisture content is 3.30%

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Abstract

The invention discloses a preparation method of memetasone furoate monohydrate, which comprises the following steps of: a, forming an organic water solution of mometasone furoate, formed by mixing water with an organic solvent, wherein the organic solvent is selected from one or more DMF (Dimethyl Formamide), DMSO (dimethylsulfoxide) and THF (tetrahydrofuran); and B, precipitating crystals from the solution obtained in the step a by using a conventional crystallizing method, wherein the conventional crystallizing method comprises a cooling method and a solvent evaporating method.

Description

Field of invention: [0001] The invention relates to a steroid drug crystallization technology, in particular to a new preparation method of mometasone furoate monohydrate. Background technique: [0002] The chemical structure of Mometasone furoate monohydrate (CAS: 141646-00-6) is as follows: [0003] [0004] Mometasone furoate is a new type of glucocorticoid derivative without fluorine, which has the characteristics of high curative effect and less adverse reactions. The currently listed products include nasal spray (trade name: Nesuna) and ointment (trade name: Ai Luo Song). Among them, Ren Xiaowei and others mentioned in Fudan Journal (Medical Edition), No. 707-710, No. 05, 2008 that the first-selected drug recommended by the World Health Organization for the treatment of allergic rhinitis in 2001 was glucocorticoids. Among them, mometasone furoate is the most representative because of its definite curative effect and small systemic adverse reactions. It can be se...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J17/00
Inventor 何运良翁路
Owner TIANJIN JINYAO GRP
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