A kind of raspberry ketone reaction device and raspberry ketone continuous preparation method
A raspberry ketone and reaction device technology, applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problems of complicated separation and purification operations, high safety risks, and low yields, and achieve heat transfer Good effect, simple production process, good effect of continuous reaction
Active Publication Date: 2021-08-31
CHENGDA PHARM CO LTD
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Problems solved by technology
Compared with other schemes, this scheme has better atom economy and is also applied in industry, but the reaction is carried out in ethanol solvent with nickel catalyst, which is very prone to further reduction reaction of carbonyl and generates by-product raspberry alcohol, so it is usually necessary to use After purification by distillation or even rectification, the product is obtained by recrystallization and purification. The separation and purification operation is complicated and the yield is not high
In addition, when the nickel catalyst is separated from the alcohol solvent, it is very easy to catch fire or even explode, which poses a greater safety risk
Method used
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Embodiment 1
[0052] 1) Preparation of 4-(3-oxo-1-butene) phenol sodium salt solution
[0053] In batching reactor one 1, add 3.28kg (12.3mol, 1.5eq) of 15% sodium hydroxide solution, add 1.0kg (8.2mol, 1.0eq) p-hydroxybenzaldehyde in batches, stir and dissolve to obtain 4-formyl Sodium phenolate salt solution. In another reactor or storage tank, add 595g (10.0mol, 1.25eq) of acetone for later use. Use two calibrated metering pumps to inject 4-formylphenol sodium brine solution and acetone into the mixer respectively. The injection speed of 4-formylphenol sodium brine solution is 32.3ml / min, and the injection speed of acetone is 6.9ml / min. ml / min. The mixed reaction solution enters the stainless steel microchannel reactor 2 with an inner diameter of 5mm and a total length of 3m at a speed of 2.0m / min, and a thorn-shaped protrusion on the inner wall. The temperature of the reactor is controlled at 40-45°C, and the reaction residence time for the 90s. The effluent was collected at the out...
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Abstract
The invention discloses a raspberry ketone reaction device and a continuous raspberry ketone preparation method, which uses 4-formylphenol sodium solution and acetone as raw materials and uses water as a solvent to carry out continuous aldehyde and ketone condensation in a microreactor Reaction, obtains the aqueous solution of 4-(3-oxo-1-butene) phenol sodium salt; This intermediate solution is not through separation, after adding catalyst, in the tubular reactor with propulsion propeller, continue to mix with hydrogen Carrying out the reaction, selectively reducing olefins to obtain an aqueous solution of raspberry ketone sodium salt, and then undergoing post-treatment operations such as neutralization and crystallization to obtain raspberry ketone; only water is used as a solvent in the synthesis process of the present invention, which improves the separation efficiency of the catalyst. Safety, the product selectivity is as high as 99%, and the raspberry alcohol produced by excessive reduction is less than 0.2%; the reaction system of the present invention has no amplification effect, has the characteristics of good continuous reaction stability, simple operation, short production cycle, simple production process, It has the advantages of less pollution and low energy consumption, and is suitable for industrial production.
Description
technical field [0001] The invention relates to the technical field of drug synthesis, in particular to a raspberry ketone reaction device and a continuous raspberry ketone preparation method. Background technique [0002] Raspberry ketone, also known as rubus ketone, chemically named 4-(4-hydroxyphenyl)-2-butanone, is a naturally occurring substance in raspberry fruit. It is a white needle-like crystal or granular solid in the form of Raspberry aroma and fruity sweetness, insoluble in water and petroleum ether, soluble in ethanol, ether and volatile oil. Raspberry ketone can be refined into spices, which can be used in both food and cosmetics. Its uses are mainly concentrated in food fixatives, modifiers, and cosmetic preparations. In recent years, studies have found that raspberry ketone has good weight-loss and blood-fat-lowering effects, and its usage in weight-loss and fat-lowering health care products has greatly increased, and it has a good market prospect. [0003]...
Claims
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IPC IPC(8): C07C45/64C07C49/245
CPCC07C45/62C07C45/64C07C45/74C07C49/245C07C49/248C07C47/565
Inventor 彭智勇施裕华陆建军钱伟刘明陈叶胡保吴凯
Owner CHENGDA PHARM CO LTD