A kind of method that catalytic oxidation mandelic acid ester prepares acetophenone ester

A technology of acetophenone ester and mandelate, which is applied in the field of catalytic oxidation of mandelate to prepare acetophenone ester, which can solve the problems of low catalytic oxidant efficiency, difficult oxidation of oxidant, and few reaction steps, etc., and achieves cheap and high-efficiency catalyst , less reaction steps and mild reaction conditions

Active Publication Date: 2021-05-25
DALIAN UNIV OF TECH
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Problems solved by technology

[0005] The purpose of the present invention is to propose a method for preparing acetophenone esters by catalytic oxidation of mandelic acid esters, aiming at the problems of low efficiency of catalytic oxidants currently used for the preparation of acetophenone esters, long reaction times, and difficult oxidation of green and environmentally friendly oxidants. The method has a simple composite catalyst formula, can be used to catalyze and oxidize mandelic acid esters to prepare acetophenone esters, and has the advantages of high catalytic efficiency, high product purity, few reaction steps, and environmental protection

Method used

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  • A kind of method that catalytic oxidation mandelic acid ester prepares acetophenone ester
  • A kind of method that catalytic oxidation mandelic acid ester prepares acetophenone ester
  • A kind of method that catalytic oxidation mandelic acid ester prepares acetophenone ester

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Embodiment 1-9

[0029] Embodiment 1-9 discloses the impact of different composite catalyst types on the conversion rate of methyl mandelic acid and the selectivity of methyl acetophenone, and the specific experimental process is described as follows:

[0030] The method for preparing acetophenone ester by catalytic oxidation of mandelic acid ester comprises the following steps: 5mmol methyl mandelate, 5mol% vanadium oxy compound, 5mol% zinc nitrate, 5ml acetonitrile is added in the 25ml reactor, after the airtight reactor, to the reactor filled with 0.2MPaO 2 , heated to 80°C under stirring, and kept for 4h, cooled to room temperature after the reaction was completed, and the product was analyzed quantitatively by gas chromatography, and the analysis results are shown in Table 1:

[0031] Table 1: Effects of different catalyst types on the conversion rate of methyl mandelate and the selectivity of methyl acetophenone

[0032]

[0033]

[0034] figure 1 For the purification product met...

Embodiment 10-14

[0036] Embodiment 10-14 discloses the impact of compounding the amount of addition of catalyst on the conversion rate of methyl mandelate and the selectivity of methyl acetophenone, and the specific experimental process is described as follows:

[0037] The method for preparing acetophenone ester by catalytic oxidation of mandelic acid ester comprises the following steps: a certain amount of catalyzer (vanadyl picolinate / zinc nitrate=100%), 5mmol methyl mandelic acid, 5ml acetonitrile is added in the 25ml reactor, to Fill the reactor with 0.2MPaO 2 , heated to 80°C under stirring, and kept for 4h, cooled to room temperature after the reaction was completed, and the product was analyzed quantitatively by gas chromatography, and the analysis results are shown in Table 2:

[0038] Table 2: Effect of catalyst addition on the conversion rate of methyl mandelate and the selectivity of methyl acetophenone

[0039]

Embodiment 15-18

[0041]Embodiment 15-18 discloses the influence of the molar ratio of transition metal nitrate and vanadium oxy compound on the conversion rate of methyl mandelate and the selectivity of methyl acetophenone, and the specific experimental process is described as follows:

[0042] The method for preparing acetophenone ester by catalytic oxidation of mandelic acid ester comprises the following steps: 5mmol methyl mandelate, 5mol% vanadyl picolinate, a certain amount of zinc nitrate, 5ml acetonitrile is added in a 25ml reactor, and the reactor is filled with 0.2MPaO 2 , heated to 80°C under stirring, and maintained for 4h, cooled to room temperature after the reaction was completed, and the product was analyzed quantitatively by gas chromatography, and the analysis results are shown in Table 3:

[0043] Table 3: The effect of the molar ratio of transition metal nitrate to vanadyl compound on the conversion of methyl mandelate and the selectivity of methyl acetophenone

[0044] ...

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Abstract

The invention belongs to the technical field of preparing acetophenone esters, and provides a method for preparing acetophenone esters by catalytically oxidizing mandelic acid esters. The component is used as a composite catalyst, and under mild reaction conditions of 30-150°C, mandelic acid ester is oxidized in one step to prepare acetophenone ester. Compared with synthetic methods such as Friedel-Crafts acylation method, benzoyl nitrile hydrolysis method and styrene oxidation method, this method has fewer reaction steps, simple operation, mild reaction conditions, environmental protection, cheap and efficient catalyst, and has a good application prospect and high practical value.

Description

technical field [0001] The invention relates to the preparation technology of acetophenone ester, in particular to a method for preparing acetophenone ester by catalytic oxidation of mandelic acid ester. Background technique [0002] Acetophenone ester, also known as benzoylformate, is a compound with a carbonyl and an ester bifunctional group and has special chemical properties. For example, methyl acetophenone is an organic intermediate and organic chemical raw material for the synthetic drug glycopyrronium bromide, pyrazine and oxazoline herbicides, fungicides and photoinitiators, and has a wide range of applications in the fields of medicine, pesticides and health care. Applications. [0003] Taking methyl acetophenone as an example, there are mainly the following methods for preparing methyl acetophenone: 1. Friedel-Crafts acylation method. The method takes aromatic compound and monoethyl oxalyl chloride as raw materials, and metered anhydrous aluminum trichloride is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/313C07C69/738B01J31/26B01J31/28B01J31/32
CPCB01J31/26B01J31/28B01J31/32C07C67/313C07C69/738
Inventor 杜中田鞠永伟宋春丽李幸霏肖楚红卢霞
Owner DALIAN UNIV OF TECH
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