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Sodium myristate crystal form and preparation method thereof

A technology of sodium myristate and crystal form, applied in the field of sodium myristate crystal form and preparation thereof, can solve the problems of cumbersome post-processing and drying, difficult product purification and the like, and achieves easy large-scale preparation, good chemical stability, Solve the effect of solvent wrapping

Active Publication Date: 2018-12-18
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The state of sodium myristate currently reported is mostly white powder or paste, and no other crystal forms have been reported.
And described these two kinds of forms have following shortcoming in the process that it prepares miplatin as drug intermediate: two kinds of forms all have certain wrapping to solvent, and this wrapping can make the impurity in the intermediate sodium myristate and The reaction of olixaplatin produces impurities, which will eventually be introduced into the final product Miplatin, resulting in cumbersome post-processing and drying, and the product is not easy to purify

Method used

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  • Sodium myristate crystal form and preparation method thereof
  • Sodium myristate crystal form and preparation method thereof
  • Sodium myristate crystal form and preparation method thereof

Examples

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Embodiment 1

[0019] Example 1: Add 5g of sodium myristate and 20ml of purified water to a 250ml reaction bottle equipped with a reflux device, heat up to 80°C, add 30ml of ethyl acetate, stir, pour the reaction solution into a 250ml beaker, and let it cool naturally 0.5h, then cool down to 5°C in an ice-water bath, stand for crystallization for 1h, collect the filter cake by suction filtration, and dry for 12h to obtain a needle-like solid in the crystal form of sodium myristate with a yield of 94.0% and a purity of 99.96%.

Embodiment 2

[0020] Example 2: Add 5g of sodium myristate and 25ml of purified water to a 250ml reaction bottle equipped with a reflux device, heat up to 70°C, add 30ml of ethyl acetate, stir, pour the reaction solution into a 250ml beaker, and let it cool naturally 0.5h, then cool down to 0°C in an ice-water bath, stand for crystallization for 1h, collect the filter cake by suction filtration, and dry for 12h to obtain a needle-like solid in the crystal form of sodium myristate, with a yield of 95.3% and a purity of 99.93%.

Embodiment 3

[0021] Example 3: Add 5g of sodium myristate and 10ml of ethanol to a 250ml reaction flask equipped with a reflux device, heat up to 80°C, add 20ml of ethyl acetate, stir, pour the reaction solution into a 250ml beaker, and let it cool naturally for 0.5 h, then cooled to 3°C in an ice-water bath, left to stand for crystallization for 1 h, collected the filter cake by suction filtration, and dried for 12 h to obtain a needle-like solid in the crystal form of sodium myristate with a yield of 94.6% and a purity of 99.91%.

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Abstract

The invention belongs to the field of chemical pharmacy, and specifically discloses a sodium myristate crystal form, which has characteristic diffraction peaks at 2[theta] angle of 4.8+ / -0.2 DEG, 6.6+ / -0.2 DEG, 7.3+ / -0.2 DEG and 12.1+ / -0.2 DEG in X-ray powder diffraction (X-RPD) with Cu-K[gamma] radiation. The invention further discloses a preparation method of the sodium myristate crystal form, wherein the preparation method comprises: dissolving sodium myristate in a protic solvent, carrying out heating dissolving, adding ethyl acetate, carrying out stirring cooling, and carrying out standing crystallization to obtain the crystal form. According to the present invention, the sodium myristate crystal form is a needle-like crystal, has characteristics of less impurities and high purity, and is not easily wrapped during the preparation of miriplatin, such that the purity of miriplatin is high, and the industrial production of miriplatin is easily achieved.

Description

technical field [0001] The invention belongs to the field of chemical industry and pharmacy, and in particular relates to a crystal form of sodium myristate and a preparation method thereof. Background technique [0002] Sodium myristate, molecular formula C 14 h 27 o 2 Na, also known as sodium myristate; soluble in water or ethanol, in terms of drug synthesis, it is a drug synthesis intermediate, which can synthesize the anticancer drug miplatin with orisaplatin. [0003] The currently reported state of sodium myristate is mostly white powder or paste, and no other crystal forms have been reported. And described these two kinds of forms have following shortcoming in the process that it prepares miplatin as drug intermediate: two kinds of forms all have certain wrapping to solvent, and this wrapping can make the impurity in the intermediate sodium myristate and The reaction of olixaplatin produces impurities, which will eventually be introduced into the final product Mip...

Claims

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Application Information

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IPC IPC(8): C07C53/126C07C51/43C07F15/00
CPCC07C51/43C07C53/126C07B2200/13C07F15/0093
Inventor 张贵民褚延军提文利
Owner LUNAN PHARMA GROUP CORPORATION
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