Preparation method for amorphous tofacitinib citrate

A technology of tofacitinib and citric acid, applied in the field of pharmacy, can solve the problems of high product impurities, reduced product purity and quality, complicated operation and the like, and achieves the effects of simple preparation method, low cost and good stability

Inactive Publication Date: 2013-05-01
BEIJING PHARMA GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented technology describes making certain chemicals called tofacitiimabcitate with improved properties such as being easier to dissolve or store at room temperatures compared to existing forms like taficamide. These improvements make it possible to produce smaller quantities while still maintaining its effectiveness over time.

Problems solved by technology

This patented technical problem addressed in this patents relates to finding an efficient way to make high-quality crystalline tofacilteimide called tofacizole citrate quickly without any unwanted substances like tacrolithium salt used during its synthesis process.

Method used

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  • Preparation method for amorphous tofacitinib citrate
  • Preparation method for amorphous tofacitinib citrate
  • Preparation method for amorphous tofacitinib citrate

Examples

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Embodiment 1

[0027] Example 1: Preparation of amorphous tofacitinib citrate (ethanol-water system) by precipitation method

[0028] Add 5g of tofacitinib citrate into the reaction flask, add 20mL of ethanol, heat to 30-35°C to completely dissolve the solid, add the solution to 20mL of 15-25°C water, and stir at 15-25°C The suspension was filtered for about 16 hours, the obtained solid was washed with ethanol / water (volume ratio 1:1), and air-dried at 60°C to constant weight to obtain 4.5 g of amorphous tofacitinib citrate with a yield of 95 %, HPLC analysis purity is 99.6%.

Embodiment 2

[0029] Example 2: Preparation of amorphous tofacitinib citrate (methanol-ethyl acetate system) by precipitation method

[0030] Add 50g of tofacitinib citrate into the reaction flask, add 100mL of methanol, heat to 30-35°C to completely dissolve the solid, add the solution to 50mL of ethyl acetate at 25-30°C, and heat at 25-30°C The resulting suspension was stirred at low temperature for about 20 hours, filtered, the obtained solid was washed with methanol / ethyl acetate (volume ratio 2:1), and air-dried at 60°C to constant weight to obtain 45.8 g of amorphous tofacitinib citrate , the yield was 91.6%, and the HPLC analysis purity was 99.7%.

Embodiment 3

[0031] Embodiment 3: Preparation of amorphous tofacitinib citrate by spray drying method

[0032] 50 g of tofacitinib citrate was dissolved in 100 mL of methanol at about 30-35° C., and the solution was spray-dried at a flow rate of about 2.5 ml / min at 30° C. to 35° C. in a nitrogen flow of 600 Nl / h. The substance was recovered from the receiver, and the obtained solid was air-dried at 60°C to constant weight to obtain 46.8 g of amorphous tofacitinib citrate, with a yield of 93.6% and a purity of 99.5% by HPLC analysis.

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Abstract

The invention provides a preparation method for amorphous tofacitinib citrate. The preparation method is simple, can easily obtain high-purity amorphous tofacitinib citrate, and is suitable for industrial application. The preparation method includes the following steps: under the temperature range between 30 DEG C and 50 DEG C, organic solvent is used for dissolving tofacitinib citrate, so that solution is produced, water which is 15 DEG C to 25 DEG C is added into the solution, so that precipitate is produced, the precipitate is put in the environment of 15 DEG C to 25 DEG C for 4 to 24 hours, and the amorphous tofacitinib citrate is then recovered.

Description

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Claims

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Application Information

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Owner BEIJING PHARMA GRP CO LTD
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