Purification method of tedizolid phosphate

A technology of tedizolid phosphate and tedizolid phosphate disodium salt, which is applied in the field of purification of tedizolid phosphate to achieve the effects of reducing waste liquid, facilitating industrial production, and improving solubility

Inactive Publication Date: 2021-06-15
HAINAN GENERAL & KANGLI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The technical problem to be solved in the present invention is to overcome the above-mentioned defects in the purification method of tedizolid phosphate in the prior art, thereby providing a purification method of tedizolid phosphate with strong impurity removal ability, simple and convenient, and beneficial to industrial production, And this method does not need to use high boiling point solvents that are difficult to remove during the purification process

Method used

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  • Purification method of tedizolid phosphate
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  • Purification method of tedizolid phosphate

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preparation example Construction

[0034] Preparation method of crude phosphate of phosphate

[0035] In a 3000 mL four round bottom flask, 1500 ml of tetrahydrofuran is added to the round bottom flask under a thermometer, and 1500 ml of tetrahydrofuran, 100 g (5R) -3- (4-bromo-3-fluorophenyl) was added to the round bottom flask under a thermometer. -5-hydroxymethazolin-2-ketone, 105 g 2- (2-methyl-2H-tetrazol-5-yl) pyridine-5-borate-borate which is alkoxide, 28 g of four (triphenylphosphine) Palladium, stirred to solid dissolve, adding a well-prepared 140 g of a small amount of water dissolved with potassium potassium carbonate solution, warmed to reflux, stirring for 12 hours, cooling to room temperature. The filter was filtered, washed with acetone after washing with water. Filter cake vacuum 45 ° C for 48 hours, 80.2 g 3- [3-fluoro-4- [6- (2-methyl-2H-Tiazol-5-yl) -3-pyridyl] phenyl] -5 (Hydroxymethyl) -2-oxazolite.

[0036] In the 2000ml three-mouth bottle, 800 ml of tetrahydrofuran was added, 80 g 3- [3-fluor...

Embodiment 1

[0039] This embodiment provides a purification method of phosphate-specific epidazole, including the following steps:

[0040] After mixing 1 g of a phosphate-deammonia-bold metal with 30 ml of anhydrous ethanol, filtered, filtered, the solid was dissolved in 12 ml of aqueous sodium hydroxide (35 wt%) to obtain aqueous phosphate-specific aqueous solution;

[0041]The pH of the aqueous solution of the phosphate-specific hydrochloric acid was adjusted with concentrated hydrochloric acid at a 100 rpm stirring rate of 2.5 h, then filtered, the solid was washed 3 times with anhydrous ethanol (15 mL), 50 ° C dry each time. 6h, ie, white powder phosphate-deammonia, yield of 81.6%.

[0042] 0.1 g of the above phosphate-specific product was 0.1 g, and 10 ml of 0.1 mol / L sodium hydroxide solution was added, followed by the clearing examination method according to the 2010 Edition of China Pharmacopoeia, and the above sodium hydroxide solution was clarified.

Embodiment 2

[0044] This embodiment provides a purification method of phosphate-specific epidazole, including the following steps:

[0045] After mixing 1 g of a phosphate-specific alkoxymide and 20 ml of anhydrous ethanol, filtered, filtered, filtered, dissolved in 15 ml of sodium hydroxide solution (25 wt%) to obtain aqueous phosphate-specific aqueous solution of sodium sodium sodium salt; 0.25 um microfiltration The membrane is filtered to filter aqueous solution of phosphatic acid species.

[0046] The pH of the aqueous solution of aqueous phosphate-deaminidide sodium salt was adjusted with concentrated hydrochloric acid, and the crystalline was crystalline at 50 rpm agitating rate, then filtered, the obtained solid was washed 3 times with anhydrous ethanol (12ml each time), 55 ° C Dry 4h, which is a white powder phosphate-deammonia product with a yield of 75.1%.

[0047] 0.1 g of the above phosphate-specific product was 0.1 g, and 10 ml of 0.1 mol / L sodium hydroxide solution was added, ...

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Abstract

The invention relates to the technical field of medicinal chemistry, in particular to a purification method of tedizolid phosphate. The method comprises the following steps: firstly, crude tedizolid phosphate is creatively mixed with absolute ethyl alcohol, impurities with lower polarity than tedizolid phosphate in the crude tedizolid phosphate are dissolved in the absolute ethyl alcohol, then the impurities are removed by filtering, and tedizolid phosphate is left in a filtered solid; and other impurities can be removed by combining the subsequent steps of converting tedizolid phosphate solid into tedizolid phosphate disodium salt, acidifying, crystallizing and the like. The tedizolid phosphate obtained through purification is high in purity, the sodium hydroxide solution is clear, and a high-boiling-point solvent which is difficult to remove does not need to be used in the purification process of the purification method. The method is simple, convenient and beneficial to industrial production.

Description

Technical field [0001] The present invention relates to the field of pharmaceutical techniques, and more particularly to a purification method of phosphate-specific azolide. Background technique [0002] Tedizolid phosphate is an oxazolidone antibiotic, which can be used to mediate protein synthesis with bacterial ribosome 50S subunit, mainly used to treat golden Staphylococcus aureus (including methoxy Western strains). , Methoxy-like-sensitive strain and various acute bacterial skin and skin structural infections caused by Gram-positive bacteria such as a variety of streptococcus and sauceurus (ABSSI). [0003] The preparation method of the existing phosphate-specific phosphate is mainly divided into the following two: I by reacting a bis (tetrabutyrate) bis (tetrabutyrate) with a sodium methoxide to give a phosphate-deammonia, which is again Acetic acid reaction, ethanol and ether crystallization, preparation. However, phosphate-specific gazolia is easily degraded under strong...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6558
CPCC07F9/65583
Inventor 彭先芬符永红钟海雄林方育肖汉文郑元女林小雪唐雄肇
Owner HAINAN GENERAL & KANGLI PHARMA
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