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Purification method of difluprednate intermediate

A technique of difluprednate and a purification method, which is applied in the field of purification of organic matter, can solve problems such as high cost, low production capacity, and difficult large-scale production, and achieve the effects of saving cost, reducing impurity content, and high yield

Pending Publication Date: 2018-09-07
广州仁恒医药科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Column chromatography is difficult to achieve large-scale production in industry, and the production capacity is low and the cost is high

Method used

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  • Purification method of difluprednate intermediate

Examples

Experimental program
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Embodiment 1

[0056] An embodiment of the purification method of the compound shown in formula I, the purification method of the compound shown in formula I described in this embodiment is: add 1.00g Na 2 SO 3 The solid was rotary evaporated at T=35°C to obtain a yellow solid, the first crude product; 4.0mL MTBE was added to the first crude product and stirred at 0°C for 30min, filtered, washed with 1.0mL MTBE, and washed with 10.0mL water to obtain White solid, the white solid was dried at T=50°C for 5h, namely the second crude product; adding isopropyl acetate and n-hexane to the second crude product to prepare a saturated solution at T=90°C, the isopropyl acetate The volume ratio to n-hexane is: isopropyl acetate: n-hexane = 7:1, then cool down to 25°C to crystallize, filter to obtain a white solid, and dry the obtained solid at T=50°C to obtain formula I compound.

[0057] The reaction yield of the obtained compound represented by formula I was 75%. According to the results of HPLC, t...

Embodiment 2

[0059] An embodiment of the purification method of the compound shown in formula I, the purification method of the compound shown in formula I described in this embodiment is: add 1.00g Na 2 SO 3 Solid, the solvent was recovered by rotary evaporation at T=35°C to obtain a yellow solid, the first crude product; add 4.0mL MTBE to the first crude product, stir at 0°C for 30min, filter, wash with 1.0mL MTBE, and wash with 10.0mL water After washing, a white solid was obtained. The white solid was dried at T=50° C. for 5 h, namely the compound represented by formula I.

[0060] The reaction yield of the obtained compound represented by formula I was 90%. According to the results of HPLC, the purity of the obtained compound represented by formula I was above 90.0%, and the maximum single heterogeneity was less than 1.0%.

Embodiment 3

[0062] An embodiment of the purification method of the compound shown in formula I, the purification method of the compound shown in formula I described in this embodiment is: add 1.00g FeCl to 1.00g of the solution containing the compound shown in formula I 2 Solid, the solvent was recovered by rotary evaporation at T=35°C to obtain a yellow solid, the first crude product; add 4.0mL MTBE to the first crude product, stir at 0°C for 30min, filter, wash with 1.0mL MTBE, and wash with 10.0mL water After washing, a white solid was obtained. The white solid was dried at T=50° C. for 5 h, namely the compound represented by formula I.

[0063] The reaction yield of the obtained compound represented by formula I was 60%. According to the results of HPLC, the purity of the obtained compound represented by formula I was above 85.0%, and the maximum single heterogeneity was less than 2.0%.

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Abstract

The invention discloses a purification method of a difluprednate intermediate. A structural formula of the difluprednate intermediate is as shown in a formula I. The purification method of the compound as shown in the formula I comprises the following steps of (1) adding a reducing agent into a solution containing the compound as shown in the formula I, removing a solvent so as to obtain a primarycoarse product; and (2) adding a beating solvent into the primary coarse product, beating, and drying to obtain the compound as shown in the formula I. In the purification method, fluoridized isomerimpurities are removed, so that less than 0.1% of isomer impurities are brought in; the processing problem after addition reaction with 1, 4-dioxane or N-bromo-succinimide of carbon tetrachloride is solved, so that the obtained coarse product can exist stably at a certain temperature without being oxidized; after purification, the compound as shown in the formula I contains less than 0.1% of eachimpurity, thereby meeting the reaction requirement of the next step; and the purification process has high yield and the cost is saved.

Description

technical field [0001] The present invention relates to a kind of purification method of organic matter, be specifically related to a kind of purification method of difluprednate intermediate. Background technique [0002] Steroids have been used to treat inflammation as a disease area for decades. Steroidal compounds with cyclopentane polyhydrophenanthrene nucleus structure combine with glucocorticoid receptors in lesion tissue cells to produce genetic and non-genetic effects, and can inhibit inflammatory trend factors and the entire process of inflammation development, thereby Achieve anti-inflammatory effect. As the earliest discovered anti-inflammatory drugs, steroid hormone drugs have comprehensive and efficient therapeutic effects on inflammation. Although there are some local or systemic side effects, they are still the most widely used anti-inflammatory drugs in clinical practice. [0003] The elimination of inflammation and pain in eye surgery is very important. A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J5/00
CPCC07J5/0053
Inventor 田元覃宇东邓琦徐显杰许志国
Owner 广州仁恒医药科技股份有限公司
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