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Catalyst and method for preparing citral by rearrangement reaction of dehydrolinalool

A technology for dehydrolinalool and citral, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve the problem of relatively expensive catalysts and molybdenum-based catalysts Resolve the problems of low activity and long reaction time, and achieve the effect of high activity and selectivity, mild reaction conditions and less dosage

Inactive Publication Date: 2018-04-27
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The activity of molybdenum-based catalysts is not high, the reaction time is long, and the catalyst price is relatively expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Put 30g (197.07mmol) of dehydrolinalool and 30g of solvent toluene into a 100mL three-necked flask equipped with a thermometer, stirrer and condenser, blow nitrogen to replace the air, and then heat to the reaction temperature of 120℃, and then add 0.96 g (3.4 mmol) isopropyl titanate, 0.18 g (1.82 mmol) cuprous chloride, and 3 g (22.03 mmol) p-toluic acid, and keep the reactor at a constant temperature until the end of the reaction. The reaction liquid was analyzed by gas chromatography, with benzyl alcohol as the internal standard substance, and the concentration of each component in the reaction liquid was calculated according to the internal standard method to calculate the conversion rate of dehydrolinalool and the yield of citral. The reaction results are listed in Table 1.

[0024] Table 1

[0025] Reaction time / hour

Embodiment 2

[0027] Reduce the amount of solvent toluene to 15g, other raw material ratios and reaction conditions are the same as in Example 1, and the reaction results are listed in Table 2.

[0028] Table 2

[0029] Reaction time / hour

Embodiment 3

[0031] 30 g of 1,2-dichlorobenzene was used as a solvent, and other raw material ratios and reaction conditions were the same as in Example 1. The reaction results are listed in Table 3.

[0032] table 3

[0033] Reaction time / hour

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PUM

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Abstract

The invention provides a combined catalyst for a hotrienol rearrangement reaction for citral preparation. The catalyst is a combination of titanium tetraisopropanolate and cuprous chloride. The invention further provides a method for preparing citral through the hotrienol rearrangement reaction which adopts the catalyst combining titanium tetraisopropanolate and cuprous chloride. The catalyst is relatively high in both activity and selectivity, low in price, easy to obtain, low in dosage and very mild in reaction condition; within a relatively short reaction time, the ideal conversion rate and yield of a target product can be obtained.

Description

Technical field [0001] The invention relates to a catalyst and a catalytic reaction method for preparing citral by using dehydrolinalool as a raw material to directly carry out a rearrangement reaction. Background technique [0002] Citral is a colorless or slightly yellow liquid with a strong lemon scent. It can be used to make citrus flavored food spices and directly used in beverage and food processing. Citral, as one of the most important open-chain monoterpenes, is a fine chemical intermediate with broad application prospects. It can be used to synthesize isopulegol, hydroxycitronellal and ionone, and can also be transformed into the production of vitamin E, An important starting material for vitamin A, isophytoalcohol or β-genone. [0003] Natural citral is found in plant essential oils such as Litsea cubeba oil, maple grass oil, lemongrass oil, eucalyptus oil, grass oil, lemon basil oil, etc. Domestic citral products are mainly extracted from plant essential oils and are li...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/30C07C45/51C07C47/21
Inventor 朱志庆赵宁波韦存茜陈卓君周卫东卢浩然
Owner EAST CHINA UNIV OF SCI & TECH
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