Dimethylamine sphaelactone-m-hydroxybenzoate as well as preparation method and application thereof

A technology of hydroxybenzoate and m-hydroxybenzoic acid, which is applied in the field of dimethylaminomildolide-m-hydroxybenzoate and its preparation, can solve the problem of poor controllability of process and product quality, and easy occurrence of crystal forms Problems such as mutual transformation and complex preparation process, etc., achieve the effect of being convenient for industrialized large-scale production and application, easy to store and transport, and simple preparation method

Active Publication Date: 2021-07-23
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to solve the existing problems of high hygroscopicity, poor stability, easy interconversion of crystal forms, complicated preparation process, strong toxicity of solvent used, and poor controllability of process and product quality in the existing dimethylamine michelolactone salt type and its preparation method and many other technical problems, the present invention provides a kind of dimethylamine michelolactone-m-hydroxybenzoate and preparation method thereof

Method used

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  • Dimethylamine sphaelactone-m-hydroxybenzoate as well as preparation method and application thereof
  • Dimethylamine sphaelactone-m-hydroxybenzoate as well as preparation method and application thereof
  • Dimethylamine sphaelactone-m-hydroxybenzoate as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Weigh 29.3 mg of dimethylaminomildolide solid and 13.8 mg of m-hydroxybenzoic acid solid, add 20 μL of ethanol, ball mill at a frequency of 20 Hz for 30 minutes, and dry at room temperature for a period of time to obtain dimethylaminomildolide-m-hydroxybenzoic acid A solid sample of salt.

[0067] figure 1 Prepare the crystallographic characteristics of the solid sample for embodiment 1, from figure 1 It can be seen that the crystallographic characteristics are: the space group is P2 1 2 1 2 1 , the cell parameters are α=90°, β=90°, γ=90°, the unit cell volume is

[0068] figure 2 For the powder X-ray diffraction pattern of the solid sample that embodiment 1 prepares, from figure 2 It can be seen that the diffraction angle is 2θ, which is expressed at 7.9°, 10.6°, 11.2°, 12.1°, 12.5°, 13.1°, 14.3°, 15.4°, 16.0°, 17.0°, 18.7°, 19.3°, 19.6°, 20.1° , 21.1°, 22.2°, 23.0°, 23.5°, 24.2°, 24.6°, 25.2°, 26.0°, 26.6°, 27.5° have characteristic peaks.

[0069] ima...

Embodiment 2

[0098] Weigh 58.6 mg of dimethylamine michelactone solid and 29.0 mg of m-hydroxybenzoic acid solid, add 50 μL of acetone, ball mill for 5 min at a frequency of 30 Hz, and dry at room temperature for a period of time to obtain dimethylamine michelactone-m-hydroxybenzoic acid solid sample.

[0099] The product that embodiment 2 obtains is carried out crystallographic test, and test result is the same as embodiment 1.

[0100] Carry out PXRD test to the product that embodiment 2 obtains, as can be known: with diffraction angle being 2θ, represent at 8.1 °, 10.8 °, 11.4 °, 12.3 °, 12.7 °, 13.3 °, 14.5 °, 15.6 °, 16.2 °, 17.2 °, There are characteristic peaks at 18.9°, 19.5°, 19.8°, 20.3°, 21.3°, 22.4°, 23.2°, 23.7°, 24.4°, 24.8°, 25.4°, 26.2°, 26.8°, 27.7°.

[0101] Carry out DSC test to embodiment 2, know: product has endothermic peak at 176.9 ℃.

[0102] Adopt the method identical with embodiment 1 to carry out following performance test by the product that embodiment 2 obtai...

Embodiment 3

[0117] Weigh 146.5 mg of dimethylamine michelactone solid and 69 mg of m-hydroxybenzoic acid solid, add 200 μL of methyl acetate, ball mill at a frequency of 25 Hz for 20 minutes, and dry at room temperature for a period of time to obtain dimethylaminomilactone-m-hydroxybenzoic acid A solid sample of salt.

[0118] The product that embodiment 3 obtains is carried out crystallographic test, and test result is the same as embodiment 1.

[0119] Carry out PXRD test to the product that embodiment 3 obtains, as can be known: take diffraction angle as 2θ to represent in 7.7 °, 10.4 °, 11.0 °, 12.0 °, 12.4 °, 12.9 °, 14.1 °, 15.2 °, 15.8 °, 16.8 °, There are characteristic peaks at 18.5°, 19.1°, 19.4°, 20.0°, 20.9°, 22.0°, 22.8°, 23.3°, 24.0°, 24.4°, 25.0°, 25.8°, 26.4°, 27.3°.

[0120] Carry out DSC test to embodiment 3, know: product has endothermic peak at 177.3 ℃.

[0121] Adopt the method identical with embodiment 1 to carry out following performance test by the product that e...

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Abstract

The invention provides dimethylamine sphaelactone-m-hydroxybenzoate as well as a preparation method and application thereof, the crystallographic characteristics of the dimethylamine sphaelactone-m-hydroxybenzoate are as follows: the space group is P212121, and the cell parameters are alpha = 90 degrees, beta = 90 degrees and gamma = 90 degrees, the dimethylamine sphaelactone-m-hydroxybenzoate prepared by the preparation method disclosed by the invention has good hygroscopicity and physical and chemical stability, and has a good drug development prospect; the preparation method is simple to operate, mild in condition, good in repeatability, green, environment-friendly, low in toxicity, safe and convenient for large-scale production and application.

Description

technical field [0001] The invention belongs to the technical field of medicine crystallization, and in particular relates to a dimethylamine michelolactone-m-hydroxybenzoate and a preparation method and application thereof. Background technique [0002] Cancer seriously endangers human life and health, with high morbidity, high mortality, and low cure rate, and has become a public health problem that has attracted much attention worldwide. According to the latest report of the World Health Organization (WHO), the incidence and death of cancer are increasing rapidly worldwide, and cancer is expected to become the leading cause of death in the 21st century. [0003] At present, the hot field of cancer drug development at home and abroad is mainly to obtain effective anticancer active ingredients from natural products. According to relevant statistics, about 1 / 4 of the world's best-selling drugs in 2015-2016 were derived from natural products and their derivatives. In recent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/93C07C65/03C07C51/43A61P35/00A61P37/06
CPCC07D307/93C07C65/03A61P35/00A61P37/06C07B2200/13
Inventor 龚俊波李中华欧阳瑞灵赵晨阳吴送姑侯宝红
Owner TIANJIN UNIV
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