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Preparation method and application of polyoxometalate crystal

A technology of heteropoly acid and crystal, which is applied in the field of preparation of heteropoly acid crystal, can solve the problems of difficult recycling and high pressure of environmental protection treatment, achieve high conversion rate and selectivity, reduce environmental pressure, and reduce production costs

Active Publication Date: 2017-07-18
山东本源晶体科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Vilanterol trifenatate (vilanterol trifenatate, chemical name ( R )-4-[2-[[6-[2-[(2,6-dichlorobenzyl)oxy]-ethoxy]hexyl]amino]-1-hydroxyethyl]-2-hydroxymethyl Phenol triphenylacetate is a new long-acting β2 receptor agonist developed by GlaxoSmithKline (GSK) for the treatment of chronic obstructive pulmonary disease and asthma; a key intermediate in the preparation of the active ingredient is ( II), formed by ring closure of the compound of formula (I) under the action of strong base potassium tert-butoxide, the yield is only 70% (see US7361787 B2 for details), and the solvent used is DMF, and the alkaline waste liquid and solvent are difficult to recover Processing, environmental protection processing pressure

Method used

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  • Preparation method and application of polyoxometalate crystal
  • Preparation method and application of polyoxometalate crystal
  • Preparation method and application of polyoxometalate crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0034] 1. Preparation of heteropolyacid crystals

[0035] 10g Na 2 WO 4 .2H 2 O and NaVO 3 .2H 2 O (with Na 2 WO 4 .2H 2 O equimolar amount) was dissolved in 100ml water and stirred to dissolve, and then disodium hydrogen phosphate (Na 2 WO 4 .2H 2 3.5 times the molar amount of O) and manganese acetate (Na 2 WO 4 .2H 2 (1.2 times the molar weight) of the aqueous solution was stirred, and after the dropwise addition, the pH was adjusted to 2.2-3.0 with sulfuric acid; 2 WO 4 .2H 2 O 4.2 times the molar amount) aqueous solution was stirred and reacted for 1-2h to obtain a turbid solution; adding potassium acetate to adjust the pH to 4.1-5.2, and a large amount of black solid was precipitated; filtering and washing the filter cake with purified water and ethanol in turn, at 40-45°C Drying; the solid obtained after drying is recrystallized with isopropyl acetate to obtain heteropolyacid crystals, and the heteropolyacid crystals are characterized by transmission elect...

Embodiment 2

[0040] With reference to the reaction process of Example 1, using the above-mentioned prepared heteropolyacid crystal as a catalyst, and using 10g (I) formula as a raw material, the reaction solvent (all of which is 7 times the weight of the substrate), reaction temperature, and heteropolyacid crystal consumption were investigated. (calculated based on the raw material (I) formula structure) on the conversion rate of (I) formula compound and the product (II) formula yield and its purity, the results are shown in Table 1:

[0041] The catalytic effect of table 1 different reaction conditions

[0042]

[0043] Note: Yield refers to the percentage of (isolation weight X purity) / theoretical yield; purity refers to the HPLC purity of the separated product, area percentage.

[0044] The above results show that the conversion rate of raw materials in ester solvents is high; at a reaction temperature of 10-15 ° C, the selectivity of raw materials is high, and the purity of products...

Embodiment 3

[0046] Using ethyl acetate as the solvent, the reaction temperature is 10-15°C, and the catalyst dosage is 2%wt. Referring to the preparation process of the compound of formula (II) in Example 1, the influence of the mechanical application of the catalyst on the reaction is investigated. The results are shown in Table 2:

[0047] Table 2 The influence of the application times of heteropolyacid crystals on the reaction

[0048]

[0049] Note: The purity of the reaction solution refers to the purity of the reaction solution after the detected reaction, not the purity of the crude product obtained after post-processing; the recovery rate of heteropoly acid crystals refers to the weight of the heteropoly acid crystals obtained by filtering and drying after the reaction and the weight of the feed before the reaction percentage.

[0050] The above results show that the conversion rate of the raw material and the selectivity of the product do not decrease significantly after the c...

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Abstract

The invention belongs to the technical field of organocatalysis and in particular relates to a preparation method and application of a polyoxometalate crystal. The preparation method disclosed by the invention comprises the following steps: by taking Na2WO4.2H2O, NaVO3.2H2O, disodium hydrogen phosphate, manganese acetate and benzyl tri-n-butylammonium chloride as raw materials, preparing the heteropolyacid crystal. Catalyzed preparation of an anti-asthma drug vilanterol trifenatate intermediate is realized by taking the polyoxometalate crystal as a catalyst. The defect in the conventional process that a strong base is adopted is overcome, the pressure for environmental protection is alleviated, the process route is green and environment-friendly, and the requirements on the conventional industrial production are met.

Description

technical field [0001] The invention belongs to the technical field of organic catalysis, and in particular relates to a preparation method and application of a heteropolyacid crystal. Background technique [0002] Heteropoly acids (Polyoxometalates, abbreviated as POMs) are composed of heteroatoms (such as P, Si, Fe, Co, etc.) and polyatoms (such as Mo, W, V, Nb, Ta, etc.) according to a certain structure through the coordination of oxygen atoms A class of oxygen-containing polyacids composed of bridges has high catalytic activity. It is not only acidic but also has redox properties. It is a multifunctional new catalyst. The heteropolyacid has good stability and can be used as a homogeneous and Heterogeneous reaction, even can be used as a phase transfer catalyst, no pollution to the environment, is a promising green catalyst, it can be used for aromatic hydrocarbon alkylation and dealkylation reaction, esterification reaction, dehydration / combination reaction , redox reac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D413/04B01J31/18B01J27/188
CPCB01J23/002B01J27/188B01J29/045B01J37/0201B01J37/08B01J2523/00C07D413/04B01J2523/51B01J2523/55B01J2523/69B01J2523/72
Inventor 赵兴亚杨志远于法鹏杨冰雪
Owner 山东本源晶体科技有限公司
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