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 quater

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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