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Method for preparing 2-methyltetrahydrofuran by taking 4-pentene-1-ol as raw material in one step through high-efficiency catalyst

A methyltetrahydrofuran, catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of poor thermal stability and oxidation resistance, easy swelling Difficult to continuously catalyze the reaction, low specific surface area, etc., to achieve the effect of easy recovery, rapid and safe separation of catalyst, and high yield

Active Publication Date: 2018-05-04
SHANGHAI LINKCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The glycol method uses pentaethoxyphosphorus as a catalyst and dichloromethane as a solvent to dehydrate 2-methyl-1,4-butanediol. This method has mild conditions, high yield, and relatively low equipment requirements. Low, but the raw materials are rare, and it is easy to cause environmental pollution, so it is difficult to promote
Organic polymers are functionalized to introduce organic functional groups, but usually the specific surface area is relatively low, the thermal stability and oxidation resistance are poor, and it is easy to swell in the organic system and difficult to continuously catalyze the reaction; while most of the inorganic carriers are cheap and easy to obtain. Good mechanical strength and thermal stability, so there are more and more researches on inorganic carrier-supported catalysts, and they also have better market prospects

Method used

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  • Method for preparing 2-methyltetrahydrofuran by taking 4-pentene-1-ol as raw material in one step through high-efficiency catalyst
  • Method for preparing 2-methyltetrahydrofuran by taking 4-pentene-1-ol as raw material in one step through high-efficiency catalyst
  • Method for preparing 2-methyltetrahydrofuran by taking 4-pentene-1-ol as raw material in one step through high-efficiency catalyst

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Embodiment

[0035] (1) Preparation of ferroferromagnetic nanoparticles wrapped in silica gel:

[0036] Take 11.0g of ferric chloride and 4.0g of ferrous chloride and dissolve them in 250mL of deionized water under nitrogen atmosphere at 85°C with vigorous stirring, then adjust the pH value to 9 with concentrated ammonia water, keep stirring for 4h, and wash the precipitate with deionized water Wash until neutral to obtain black ferric oxide particles (8-12nm). Take 2.0g of the above iron ferric oxide particles and ultrasonicate at room temperature for 30min, disperse in 400mL ethanol, then add 12mL concentrated ammonia water and 4.0mL tetraethyl orthosilicate, stir and react for 24h, the black precipitate is magnetically separated and washed with ethanol several times Vacuum drying after neutrality, obtained silica gel-wrapped ferroferric oxide magnetic nanoparticles (20-30nm), such as figure 1 shown.

[0037] (2) Preparation of 3-azidopropyltriethyloxysilane:

[0038] In a 150mL round...

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Abstract

The invention discloses a method for preparing 2-methyltetrahydrofuran by taking 4-pentene-1-ol as a raw material in one step through a high-efficiency catalyst. The 2-methyltetrahydrofuran is prepared by taking the 4-pentene-1-ol as the raw material, catalyzing through a magnetic loaded cation lanthanum series complex catalyst and carrying out intramolecular hydrogen alkylation; the magnetic loaded cation lanthanum series complex catalyst is obtained by connecting a cation lanthanum series complex and hydroxyl on the surface of a functionalized magnetic nano-carrier; the functionalized magnetic nano-carrier is obtained by carrying out surface silanization treatment on silica sol covered ferroferric oxide nanoparticles. According to the method disclosed by the invention, the catalyst doesnot contain noble metal; the method has the advantages of low preparation cost, low reaction pressure and moderate temperature which is about 80 DEG C, and has the characteristics of simplicity and convenience for operation, high yield, low byproducts, easiness for recycling the catalyst and the like, so that an efficient and green synthesis method for rapidly and safely separating the catalyst isrealized.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for synthesizing 2-methyltetrahydrofuran. Background technique [0002] 2-Methyltetrahydrofuran is an important organic intermediate and an excellent solvent. In organic synthesis, it is mainly used in the synthesis of chloroquine phosphate, primaquine phosphate and thiamine. At the same time, because it has a moderate boiling point (80.2°C), low solubility in water, easy separation from water, and similar Lewis basicity to tetrahydrofuran (THF), it can be applied to many organometallic reactions. It is superior to the current "universal solvent" tetrahydrofuran, enabling it to develop rapidly in the field of solvent replacement applications: (1) used to replace tetrahydrofuran, ether, etc., which have great safety hazards, as Grignard reaction reagents; (2) used to replace high Toxic halogenated hydrocarbons, benzene, etc. are used as reaction reagents or extraction s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/06B01J31/28
CPCB01J31/28B01J2231/4288C07D307/06Y02P20/584
Inventor 陆茜
Owner SHANGHAI LINKCHEM TECH CO LTD
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