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Novel crystal form of tedizolid phosphate disodium salt and preparation method of novel crystal form

A technology of tedizolid phosphate disodium salt and crystal form, which is applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., and can solve the problems of unstable properties, high production costs, and refining effects. Poor and other problems, achieve good particle size and stability, facilitate subsequent processing operations, and good stability

Inactive Publication Date: 2015-04-29
QILU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the existing patent literature also discloses the preparation method of this intermediate, the steps are cumbersome, the operation cycle is long, the refining effect is poor, the production cost is high, the yield is low, and the property is unstable

Method used

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  • Novel crystal form of tedizolid phosphate disodium salt and preparation method of novel crystal form
  • Novel crystal form of tedizolid phosphate disodium salt and preparation method of novel crystal form
  • Novel crystal form of tedizolid phosphate disodium salt and preparation method of novel crystal form

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042]Example 1 Preparation of tedizolid phosphate disodium salt crystal form I:

[0043] Put 100mg of tedizolid phosphate disodium salt into a 50ml reaction bottle, add 1ml of water, stir to dissolve, then add 3ml of methanol dropwise, filter with suction after precipitation, wash with a mixed solvent of water and methanol (volume ratio 1:1), wash for 40 After vacuum drying at °C for 6 hours, 69 mg of needle-like crystals were obtained, which was Form I, with a yield of 69.0%;

[0044] After determination, its X-RPD pattern is as follows figure 1 As shown, its DSC-TGA spectrum is as figure 2 shown.

[0045] 1H-NMR (600MHz, DMSO, δppm): 3.59(d,1H), 3.72(d,1H), 3.92(t,1H), 4.15(t,1H), 4.49(s,3H), 5.28(s, 1H), 7.52(d, 1H), 7.65(m, 2H), 8.25(dd, 2H), 8.93(s, 1H).

Embodiment 2

[0046] Example 2 Preparation of crystal form I of tedizolid phosphate disodium salt:

[0047] Put 100mg of tedizolid phosphate disodium salt into a 50ml reaction bottle, add 1ml of water, stir to dissolve, then add 4.5ml of ethanol dropwise, filter with suction after precipitation, and wash with a mixed solvent of water and ethanol (10:10 by volume) The filter cake was vacuum-dried at 40°C for 6 hours to obtain 72 mg of needle-like crystals, with a yield of 72.0%;

[0048] After determination, its X-RPD pattern and figure 1 Basically the same, its DSC-TGA spectrum and figure 2 Basically the same.

Embodiment 3

[0049] Example 3 Preparation of crystal form I of tedizolid phosphate disodium salt:

[0050] Put 100mg of tedizolid disodium phosphate into a 50ml reaction bottle, add 1ml of water, stir to dissolve, then add 4ml of acetonitrile dropwise, filter with suction after precipitation, wash and filter with a mixed solvent of water and acetonitrile (10:10 by volume) The cake was vacuum-dried at 40°C for 6 hours to obtain 65 mg of needle-like crystals, with a yield of 65.0%;

[0051] After determination, its X-RPD pattern and figure 1 Basically the same, its DSC-TGA spectrum and figure 2 Basically the same.

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Abstract

The invention belongs to the field of medical chemistry and particularly relates to a novel crystal form of tedizolid phosphate disodium salt with efficient antibacterial activity and a preparation method of the novel crystal form. The novel crystal form has good fluidity and repeatability and is convenient to separate and store; the defects that tedizolid phosphate disodium salt is poor in degree of crystallinity and is inconvenient to separate and store in the prior are overcome.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a new crystal form of tedizolid phosphate disodium salt with high-efficiency antibacterial activity, and discloses a preparation method thereof. Background technique [0002] Tedizolid phosphate, the chemical name is (R)-3-(4-(2-(2-methyltetrazol-5-yl)pyridin-5-yl)-3-fluorophenyl)- 5-Hydroxymethyloxazolidin-2-one dihydrogen phosphate is a second-generation oxazolidinone antibiotic developed by Dong-A Pharmaceutical and licensed to Cubist Pharmaceuticals and Bayer for commercial development. The drug inhibits protein synthesis by binding to the 50S subunit of the bacterial ribosome, and was approved by the FDA in the United States on June 20, 2014. It is mainly used for the treatment of Staphylococcus aureus (including methicillin-resistant strains) , methicillin-susceptible strains) and acute bacterial skin and skin structure infections (ABSSSI) caused by Gram-posi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6558
Inventor 张明会刘振李书彬王万远王新胜侯贺增
Owner QILU PHARMA
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