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A kind of environment-friendly synthetic method of p-methoxybenzaldehyde

A technology of p-methoxybenzaldehyde and p-hydroxybenzaldehyde, which is applied in the field of synthesis of p-methoxybenzaldehyde, can solve the problems of poisonous and harmful use, difficult post-processing, low synthesis yield, etc.

Active Publication Date: 2021-04-09
山东达冠科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0022] The purpose of the present invention is to address the low synthesis yield of p-methoxybenzaldehyde in the prior art, the use of toxic and harmful, or flammable and explosive raw materials as methylation reagents, or the use of quaternary ammonium salts that are easily decomposed by heat for phase transfer Problems such as post-processing difficulties caused by catalysis, provide a green, efficient, and economically feasible method for synthesizing p-methoxybenzaldehyde

Method used

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  • A kind of environment-friendly synthetic method of p-methoxybenzaldehyde

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Experimental program
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Effect test

Embodiment 1

[0042] 61g p-hydroxybenzaldehyde, 100mL DMC, 300mL H 2 O, 2g NaY (1:1 compound) complex and 1g Turkish red oil were added to the pressure-resistant reactor together, stirred and heated, and when the reaction temperature reached 160°C, the timing was started, and the reaction temperature was controlled to react at 160°C for 3 hours , then cooling, solid-liquid separation and liquid-liquid separation, the filtrate is fractionated and concentrated to reclaim the solvent, the concentrated solution is detected by gas chromatography and its content is 99.2%, and the calculated p-methoxybenzaldehyde yield is 96.3%.

Embodiment 2

[0044] 122g p-hydroxybenzaldehyde, 200mL DMC, 600mL H 2 O. Add 4g NaY (1:1 compound) compound and 2g Turkish red oil into the pressure-resistant reactor together, stir and heat, start timing when the reaction temperature reaches 160°C, control the reaction temperature at 160°C for 3h , then cooling, solid-liquid separation and liquid-liquid separation, the filtrate is fractionated and concentrated to reclaim the solvent, the concentrated solution is detected by gas chromatography and the calculated p-methoxybenzaldehyde yield is 97.3%.

Embodiment 3

[0046] Repeat the operation of Example 2, the added water is taken from the separated mother liquor after the reaction of Example 2, no new catalyst is added, and the p-methoxybenzaldehyde yield is calculated to be 97.4%.

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Abstract

The invention relates to an environment-friendly synthesis method of p-methoxybenzaldehyde, which uses p-hydroxybenzaldehyde as a raw material, uses polar solvent water as a solvent in the temperature range of 130-180°C, and uses Y-type zeolite, an alkaline substance, as a solvent. Catalyst, and add appropriate surfactant Turkish red oil to make emulsifier etc. under specific conditions, prepare p-methoxybenzaldehyde with environment-friendly dimethyl carbonate (DMC) as methylation raw material, and its yield reaches more than 96% , The purity of the final product reaches more than 99%.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a synthesis method of p-methoxybenzaldehyde. Background technique [0002] p-Methoxybenzaldehyde is also known as anisaldehyde and anisaldehyde, and its scientific name is 4-methoxybenzaldehyde. It has a long-lasting aroma of hawthorn, and it is a colorless oily liquid at room temperature. The main spice is used as a modifier in sweet-scented osmanthus essence; it can also be used in daily flavors and food flavors, and it works well with essential oils such as tangerine; it is also an important intermediate in organic synthesis, and it is an antimicrobial drug called hydroxylamine The intermediate of carbapenicillin is also the intermediate for the synthesis of porphyrin photosensitizers; it is also used as a fluorescent probe for the determination of nucleic acid and other biomacromolecules; it is also an excellent brightener for cyanide-free zinc plating DE additives, and can ...

Claims

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Application Information

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IPC IPC(8): C07C45/64C07C47/575
CPCC07C45/64C07C47/575
Inventor 徐志华张永富张健雄杨丰科姜云兵
Owner 山东达冠科技有限责任公司
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