A kind of preparation method of high-purity chiral inositol
By using a mixed hydrolysis method of lentizolicin hydrochloride and hydrochloric acid in the preparation of D-chinositol, combined with calcium oxide post-treatment and a molybdenum disulfide catalyst supported by platinum and praseodymium, the problems of large amount of ion exchange resins and low purity of D-chinositol in the prior art were solved, and the preparation of D-chinositol with high purity and high yield was achieved, reducing the process cost.
Patent Information
- Application Number
- CN202510010085.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-03
- Publication Date
- 2025-04-04
AI Technical Summary
In the prior art, when D-chinositol is prepared using lysyringin hydrochloride as raw material, the amount of ion exchange resin is used, resulting in a low purity of D-chinositol and a high process cost.
The mixture of lemtomycin hydrochloride and hydrochloric acid was used for hydrolysis, and post-treatment was performed by calcium oxide, and the molybdenum disulfide supported by platinum and praseodymium was used as a catalyst to reduce the amount of ion exchange resin and improve the yield and purity of D-chinositol.
The amount of ion exchange resin is significantly reduced, the purity and yield of D-chinositol are improved, and the process cost is reduced.
Smart Images
Figure CN119751207A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of preparation of chiro-inositol, and specifically to a method for preparing high-purity chiro-inositol. Background Art
[0002] There are chiral carbon atoms in the molecules of chiral inositol, and there are two optical isomers, L-configuration and D-configuration. Among them, D-chiro-inositol has biological activity, and has antioxidant, anti-inflammatory, hypoglycemic and other functions, and is widely used in the medical field. The sources of D-chiro-inositol are mainly the following: one is to extract it from natural products, such as: D-chiro-inositol can be obtained by extraction from bitter buckwheat, but the yield and purity of D-chiro-inositol obtained by this method are not ideal; the second is to obtain it through chemical synthesis, mostly using halogenated benzene as raw materials to prepare D-chiro-inositol, but the product yield is low and the synthesis route is cumbersome.
[0003] Another method for obtaining D-chiro-inositol is to prepare D-chiro-inositol by hydrolysis with trifluoroacetic acid or hydrochloric acid using kasugamycin hydrochloride. Although the process of this method is relatively simple, a large amount of hydrochloric acid needs to be added during hydrolysis, resulting in excessive chloride ions in the hydrolyzate, affecting the yield and purity of D-chiro-inositol. Meanwhile, the existing process is to remove chloride ions by a large amount of expensive ion exchange resins after concentrating and removing a part of hydrochloric acid, and there is a problem of high cost. Therefore, a method for preparing chiro-inositol is needed, and kasugamycin hydrochloride is used as a raw material to prepare D-chiro-inositol to reduce the yield and purity of chiro-inositol while reducing ion exchange resins. Summary of the invention
[0004] The invention provides a method for preparing high-purity chiro-inositol, which solves the problems in the related art that a large amount of ion exchange resin is used and the purity of D-chiro-inositol is low when preparing D-chiro-inositol using kasugamycin hydrochloride as a raw material.
[0005] The technical solution of the present invention is as follows: The present invention provides a method for preparing high-purity chiro-inositol, comprising the following steps: S1, mixing and hydrolyzing kasugamycin hydrochloride and hydrochloric acid to obtain a mixed solution; S2, concentrating the mixed solution, cooling it, adding calcium oxide for mixed reaction, using ion exchange resin for desalting and impurity removal, collecting the flow-through liquid, and drying it to obtain D-chiro-inositol.
[0006] As a further technical solution, in step S2, methanol is added after the mixed reaction for separation, and the solid product is collected and dissolved in pure water.
[0007] As a further technical solution, concentration and crystallization treatments are also performed before drying; A catalyst is also added during the mixed hydrolysis; The mass of the catalyst is 1% to 2% of the mass of the kasugamycin hydrochloride.
[0008] As a further technical solution, the temperature of the mixed reaction is 40-60°C and the time is 30-50 minutes.
[0009] As a further technical solution, the concentration temperature is 85-95°C and the time is 3-4h.
[0010] As a further technical solution, the concentration of the hydrochloric acid is 5~8mol / L.
[0011] As a further technical solution, the mass volume ratio of kasugamycin hydrochloride and hydrochloric acid is 1-4 g:10 mL; The mass ratio of the kasugamycin hydrochloride to the calcium chloride is 1-4:5.
[0012] As a further technical solution, the catalyst comprises a molybdenum disulfide matrix and a supporting component; The supported components include platinum and praseodymium.
[0013] In the present invention, chiral inositol is prepared by hydrolyzing kasugamycin hydrochloride with hydrochloric acid, and molybdenum disulfide loaded with platinum and praseodymium is used as a catalyst, thereby further improving the yield and purity of D-chiral inositol.
[0014] As a further technical solution, the precursor of praseodymium is one of praseodymium nitrate and praseodymium acetate; the precursor of platinum is platinum nitrate.
[0015] As a further technical solution, the mass ratio of the molybdenum disulfide matrix, the praseodymium precursor and the platinum precursor is 3~5:2:1.
[0016] In the present invention, when the mass ratio of the molybdenum disulfide matrix, the praseodymium precursor and the platinum precursor during catalyst preparation is 3-5:2:1, the yield and purity of D-chiro-inositol are further improved.
[0017] As a further technical solution, the method for preparing the catalyst comprises the following steps: A1, mixing a praseodymium precursor, a platinum precursor and water to obtain a precursor solution; A2. Immersing the molybdenum disulfide substrate in the precursor solution and calcining it under an inert atmosphere to obtain a catalyst.
[0018] The working principle and beneficial effects of the present invention are: In the present invention, chiro-inositol is prepared by hydrolyzing kasugamycin hydrochloride with hydrochloric acid, and calcium oxide is used to post-treat the hydrolyzate, thereby significantly reducing the amount of ion exchange resin and improving the purity of D-chiro-inositol. BRIEF DESCRIPTION OF THE DRAWINGS
[0019] The present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments.
[0020] Figure 1 The liquid chromatogram of D-chiro-inositol prepared in Example 9 of the present invention. DETAILED DESCRIPTION
[0021] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0022] In the following examples and comparative examples, the model of the ion exchange resin is IRC120H.
[0023] Example 1 The preparation method of high-purity chiro-inositol comprises the following steps: S1, mixing and hydrolyzing kasugamycin hydrochloride and hydrochloric acid to obtain a mixed solution; S2, the mixed solution was concentrated, cooled, 5g of calcium oxide was added for mixed reaction, the pH was adjusted to neutral, 5 volumes of methanol were added for purification, the solid was collected and dissolved in 20mL of pure water, 10g of ion exchange resin was used for desalination, the permeate was collected, vacuum concentrated, crystallized, and dried to obtain D-chiro-inositol; The mixing temperature is 50°C and the time is 40 min; the concentration temperature is 90°C and the time is 3 h; the concentration of hydrochloric acid is 6 mol / L; and the mass volume ratio of kasugamycin hydrochloride and hydrochloric acid is 3 g:10 mL.
[0024] Example 2 The preparation method of high-purity chiro-inositol comprises the following steps: S1, mixing and hydrolyzing kasugamycin hydrochloride and hydrochloric acid to obtain a mixed solution; S2, the mixed solution was concentrated, cooled, 5g of calcium oxide was added for mixed reaction, the pH was adjusted to neutral, 5 volumes of methanol were added for pure analysis, the solid was collected and dissolved in 20mL of pure water, 10g of ion exchange resin was used for elution, the permeate was collected, vacuum concentrated, crystallized, and dried to obtain D-chiro-inositol; The mixing temperature is 40°C and the time is 30 min; the concentration temperature is 85°C and the time is 4 h; the concentration of hydrochloric acid is 8 mol / L; and the mass volume ratio of kasugamycin hydrochloride and hydrochloric acid is 1 g:10 mL.
[0025] Example 3 The preparation method of high-purity chiro-inositol comprises the following steps: S1, mixing and hydrolyzing kasugamycin hydrochloride and hydrochloric acid to obtain a mixed solution; S2, the mixed solution was concentrated, cooled, 5g of calcium oxide was added for mixed reaction, the pH was adjusted to neutral, 5 volumes of methanol were added for pure analysis, the solid was collected and dissolved in 20mL of pure water, 10g of ion exchange resin was used for elution, the permeate was collected, vacuum concentrated, crystallized, and dried to obtain D-chiro-inositol; The mixing temperature is 60°C and the time is 50 min; the concentration temperature is 95°C and the time is 3 h; the concentration of hydrochloric acid is 5 mol / L; and the mass volume ratio of kasugamycin hydrochloride and hydrochloric acid is 4 g:10 mL.
[0026] Example 4 The only difference between this embodiment and embodiment 3 is that a catalyst is added during the mixed hydrolysis in step S1, and the mass of the catalyst is 1% of the mass of kasugamycin hydrochloride; The method for preparing a catalyst comprises the following steps: A1. Mixing praseodymium nitrate and water to obtain a precursor solution; A2, immersing the molybdenum disulfide substrate in a precursor solution and calcining it under an inert atmosphere to obtain a catalyst; The mass ratio of molybdenum disulfide matrix and praseodymium nitrate is 2:2.
[0027] Example 5 The only difference between this embodiment and embodiment 3 is that a catalyst is added during the mixed hydrolysis in step S1, and the mass of the catalyst is 1% of the mass of kasugamycin hydrochloride; The method for preparing a catalyst comprises the following steps: A1. Mixing platinum nitrate and water to obtain a precursor solution; A2, immersing the molybdenum disulfide substrate in a precursor solution and calcining it under an inert atmosphere to obtain a catalyst; The mass ratio of molybdenum disulfide matrix and platinum nitrate is 2:1.
[0028] Example 6 The difference between this embodiment and embodiment 5 is only the preparation method of the catalyst, which comprises the following steps: A1. Mixing platinum nitrate, praseodymium nitrate and water to obtain a precursor solution; A2, immersing the molybdenum disulfide substrate in a precursor solution and calcining it under an inert atmosphere to obtain a catalyst; The mass ratio of molybdenum disulfide matrix, praseodymium nitrate and platinum nitrate is 2:2:1.
[0029] Example 7 The only difference between this embodiment and embodiment 6 is that the mass ratio of molybdenum disulfide matrix, praseodymium nitrate and platinum nitrate is 6:2:1.
[0030] Example 8 The only difference between this embodiment and embodiment 6 is that the mass ratio of molybdenum disulfide matrix, praseodymium nitrate and platinum nitrate is 5:2:1.
[0031] Example 9 The only difference between this embodiment and embodiment 6 is that the mass ratio of molybdenum disulfide matrix, praseodymium nitrate and platinum nitrate is 3:2:1.
[0032] Comparative Example 1 The difference between this comparative example and Example 3 is only that no calcium chloride is added.
[0033] Comparative Example 2 The difference between this comparative example and Example 3 is that calcium chloride is not added, and 50 g of ion exchange resin is added.
[0034] The yield and purity of the D-chiro-inositol obtained in Examples 1 to 9 and Comparative Examples 1 to 2 were tested respectively, and the results are shown in Table 1 below.
[0035] Table 1 Test results
[0036] Compared with Comparative Examples 1 to 2, the purity of D-chiro-inositol obtained in Examples 1 to 9 is higher, indicating that the chiro-inositol is prepared by the method of hydrolysis with kasugamycin hydrochloride and hydrochloric acid, and the hydrolyzate is post-treated with calcium oxide, which significantly reduces the amount of ion exchange resin used and improves the purity of D-chiro-inositol.
[0037] Compared with Examples 4 to 5, the purity and yield of D-chiro-inositol obtained in Examples 6 to 9 are higher, indicating that the chiro-inositol is prepared by the method of hydrolysis with kasugamycin hydrochloride and hydrochloric acid, and the catalyst is molybdenum disulfide loaded with platinum and praseodymium, which further improves the yield and purity of D-chiro-inositol.
[0038] Compared with Examples 6 to 7, the purity and yield of D-chiro-inositol obtained in Examples 8 to 9 are higher, indicating that when the mass ratio of the molybdenum disulfide matrix, the praseodymium precursor and the platinum precursor during catalyst preparation is 3 to 5:2:1, the yield and purity of D-chiro-inositol are further improved.
[0039] The liquid chromatogram of D-chiro-inositol obtained in Example 9 is as follows: Figure 1 As shown; Figure 1 In the analysis, the retention time of the characteristic peak of D-chiro-inositol was 10.420 min, and the peak width was 1.32 min.
[0040] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.
Claims
1. A method for preparing high-purity chiro-inositol, characterized in that: The following steps are involved: S1, mixing and hydrolyzing kasugamycin hydrochloride and hydrochloric acid to obtain a mixed solution; S2, concentrating the mixed solution, cooling it, adding calcium oxide for mixed reaction, removing impurities with ion exchange resin, collecting the flow-through, and drying to obtain D-chiro-inositol.
2. A method for preparing high-purity chiro-inositol according to claim 1, characterized in that: In step S1, a catalyst is also added during the mixed hydrolysis; The mass of the catalyst is 1% to 2% of the mass of the kasugamycin hydrochloride.
3. A method for preparing high-purity chiro-inositol according to claim 1, characterized in that, The temperature of the mixed reaction is 40-60° C. and the time is 30-50 min.
4. A method for preparing high-purity chiro-inositol according to claim 1, characterized in that: The concentration temperature is 85-95° C. and the concentration time is 3-4 hours.
5. A method for preparing high-purity chiro-inositol according to claim 1, characterized in that: The concentration of the hydrochloric acid is 5-8 mol / L.
6. A method for preparing high-purity chiro-inositol according to claim 5, characterized in that: The mass volume ratio of kasugamycin hydrochloride and hydrochloric acid is 1-4 g:10 mL; The mass ratio of the kasugamycin hydrochloride to the calcium chloride is 1-4:
5.
7. A method for preparing high-purity chiro-inositol according to claim 2, characterized in that: The catalyst comprises a molybdenum disulfide matrix and a supporting component; The supported components include platinum and praseodymium.
8. A method for preparing high-purity chiro-inositol according to claim 7, characterized in that: The precursor of praseodymium is one of praseodymium nitrate and praseodymium acetate; the precursor of platinum is platinum nitrate.
9. A method for preparing high-purity chiro-inositol according to claim 8, characterized in that: The mass ratio of the molybdenum disulfide matrix, the praseodymium precursor and the platinum precursor is 3-5:2:
1.
10. A method for preparing high-purity chiro-inositol according to claim 9, characterized in that: The method for preparing the catalyst comprises the following steps: A1, mixing a praseodymium precursor, a platinum precursor and water to obtain a precursor solution; A2. Immersing the molybdenum disulfide substrate in the precursor solution and calcining it under an inert atmosphere to obtain a catalyst.