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Method for preparing 3-methyl-2-butenol through photocatalysis

A butenol and photocatalytic technology, which is applied in the fields of isomerization preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of difficult product separation, reduced yield, high cost, etc., and achieves low energy consumption. , Simple operation, mild reaction conditions

Active Publication Date: 2020-12-25
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This route is a hydroisomerization reaction that occurs in the presence of hydrogen. It is easy to produce isoamyl alcohol as a by-product of hydrogenation, which is difficult to separate from the product, resulting in a decrease in yield.
[0007] CN 103861633 discloses a method for preparing 3-methyl-2-buten-1-ol with a heterogeneous catalyst. The catalyst is composed of metals such as Pd, Au, Pt, and Mo. In the reaction, the overhydrogenated product isopentyl The alcohol content has been greatly reduced to 0.8%, and the cost of its separation and removal is still very expensive

Method used

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  • Method for preparing 3-methyl-2-butenol through photocatalysis
  • Method for preparing 3-methyl-2-butenol through photocatalysis
  • Method for preparing 3-methyl-2-butenol through photocatalysis

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Under an oxygen-free and water-free atmosphere, 258.6g tetrahydrofuran and 86.2g (1.0mol) 3-methyl-3-butenol were added to the photochemical reactor, and then an inert gas was passed into the reactor, and 75.96mg ( 0.5mmol) lithium hexafluorophosphate (0.05mol% relative to 3-methyl-3-butenol), start stirring until the solution is mixed and clear, then keep the temperature at 0°C, turn on the mercury lamp in the reactor, and control the wavelength to 650nm, After irradiating with a power of 350W for 8h, the conversion rate was determined to be 97% by calibrated GC analysis, the selectivity of 3-methyl-2-butenol was 99.9%, and the formation of isoamyl alcohol was not detected.

Embodiment 2

[0041]Under an oxygen-free and water-free atmosphere, 1551.6g tetrahydrofuran and 172.4g (2.0mol) 3-methyl-3-butenol were added to the photochemical reactor, and then an inert gas was passed into the reactor, and 18.75mg ( 0.2mmol) lithium tetrafluoroborate (0.01mol% relative to 3-methyl-3-butenol), start stirring until the solution is mixed and clear, then keep the temperature at -10°C, turn on the mercury lamp in the reactor, and control The wavelength is 550nm, and the power of 350W is irradiated for 12h. The conversion rate is 96% and the selectivity of 3-methyl-2-butenol is 99.9% as determined by calibrated GC analysis. The formation of isoamyl alcohol is not detected.

Embodiment 3

[0043] Under an oxygen-free and water-free atmosphere, 344.8g tetrahydrofuran, 86.2g (1.0mol) 3-methyl-3-butenol were added to the photochemical reactor, and then an inert gas was passed into the reactor, and 193.8mg ( 1.0mmol) lithium dioxalate borate (0.1mol% relative to 3-methyl-3-butenol), start stirring until the solution is mixed and clear, then keep the temperature at 5°C, turn on the mercury lamp in the reactor, and control the wavelength The concentration was 400 nm, irradiated with a power of 350 W for 6 h, and the conversion rate was determined to be 94% by calibrated GC analysis, the selectivity of 3-methyl-2-butenol was 99.9%, and the formation of isoamyl alcohol was not detected.

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Abstract

The invention discloses a method for preparing 3-methyl-2-butenol through photocatalysis. The 3-methyl-3-butenol is efficiently subjected to isomerization reaction through photocatalysis reaction to obtain the 3-methyl-2-butenol. The method solves the problem of generation of isoamyl alcohol in the traditional preparation process of 3-methyl-2-butenol, and has the advantages of mild reaction conditions, simple operation, high product yield and easy separation.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for preparing 3-methyl-2-butenol from 3-methyl-3-butenol through photocatalytic isomerization. [0002] technical background [0003] 3-Methyl-2-butenol, also known as isopentenol, is an important intermediate in organic synthesis, which can be used to produce a variety of fine chemicals and pharmaceuticals, including citral, isophytyl alcohol, and peretinic acid In addition, it can also be used as a raw material for synthetic rubber and other organic synthetic raw materials. [0004] CN 107141197 discloses a catalyst system comprising a carbonyl iron compound, an organic base and an epoxy ligand for the isomerization of 3-methyl-3-butenol to prepare 3-methyl-2-butenol, The preparation process of the catalyst required by this reaction system is complicated and the cost is high. [0005] CN 101391939 discloses a technical route for preparing 3-methyl-2-butenol....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/03C07C29/56B01J27/18
CPCC07C29/56B01J27/1806C07C33/03
Inventor 李康张永振董菁黎源孙文龙
Owner WANHUA CHEM GRP CO LTD