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Method of synthesizing arbutin by using solid superacid as catalyst

A solid superacid and catalyst technology, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc. It can solve the problems of a large amount of waste acid, expensive reagents, and inability to repeat applications.

Active Publication Date: 2019-10-18
和德化学(苏州)有限公司
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Problems solved by technology

In the dehydration reaction of the key intermediate of synthetic arbutin in the current process route, the dehydrating agent used is boron trifluoride ether, which is inflammable and explosive, and is not suitable for industrial applications. At the same time, this type of reagent is expensive and cannot Apply mechanically repeatedly, these are all unfavorable for adopting this route to carry out large-scale production, another class of dehydrating agent is sulfuric acid, the strong acid of p-toluenesulfonic acid, when using this type of dehydrating agent, reaction selectivity is poor, and yield is very low, produces a large amount of simultaneously Waste acid is facing great environmental pressure, which runs counter to the development direction of environmentally friendly green chemistry

Method used

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  • Method of synthesizing arbutin by using solid superacid as catalyst
  • Method of synthesizing arbutin by using solid superacid as catalyst
  • Method of synthesizing arbutin by using solid superacid as catalyst

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specific Embodiment example 1

[0035] A kind of method adopting solid superacid as catalyst synthetic arbutin, it comprises the steps:

[0036]S1, preparation of solid superacid catalyst: Dissolve 20g of FeCl3 in 200g deionized water, add 100g of ammonia precipitation agent, and precipitate at room temperature for 12hrs to obtain Fe(OH)3 sol, which is filtered, washed with 20g deionized water, and washed with 100- After drying at 120°C, cool down to room temperature, impregnate with 100ml of 2.5mol / L sulfuric acid solution, filter and dry, bake at 300-500°C for 8-20hrs after drying, and then cool down to room temperature in a dry nitrogen environment to obtain a brown catalyst About 22g;

[0037] S2, preparation of intermediate Arb-1: Add 120g of acetic anhydride and 12g of sodium acetate into the reaction kettle in turn, stir and heat up to 60-80°C, add 40g of glucose in 3 batches, control the reaction temperature ≤ 100°C, after the addition is complete Control the temperature at 120-125°C for reaction an...

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Abstract

A dehydrant for a dehydration reaction of a key intermediate for synthesizing arbutin in the existing technical route is boron trifluoride diethyl etherate; ether belongs to a flammable and explosivearticle; another dehydrant is strong acid such as sulfuric acid and p-toluenesulfonic acid; such dehydrant is poor in reaction selectivity and very low in yield, generates much waste acid at the sametime and causes very high environmental protection pressure. For that reason, the invention provides a method of synthesizing arbutin by taking solid superacid as a catalyst. The method comprises thefollowing steps: preparing a solid superacid catalyst, preparing an intermediate Arb-1 by using the solid superacid as the catalyst, preparing an intermediate Arb-2 from Arb-1 by using the solid superacid as the catalyst, recovering and activating the catalyst, and performing reaction and purification using the intermediate Arb-2, methanol and sodium methoxide to form arbutin. The method has the advantages that the method causes little waste gas, waste water and industrial residue, and is green, environmentally friendly, simple and convenient in technical operation and suitable for industrialization.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for preparing a fine chemical product arbutin, and more specifically to a method for synthesizing arbutin by using a solid superacid as a catalyst. Background technique [0002] Arbutin, also known as arbutin, is white needle crystal or powder. Extracted from the leaves of bearberry, it can prevent the production of melanin by inhibiting the activity of tyrosinase in the body, thereby reducing skin pigmentation, removing spots and freckles, and also has the effect of sterilization and anti-inflammation. It is mainly used in the preparation of advanced cosmetics. In the dehydration reaction of the key intermediate of synthetic arbutin in the current process route, the dehydrating agent used is boron trifluoride ether, which is inflammable and explosive, and is not suitable for industrial applications. At the same time, this type of reagent is expensive and cannot Apply...

Claims

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Application Information

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IPC IPC(8): C07H15/203C07H1/00B01J27/053
CPCC07H15/203C07H1/00B01J27/053Y02P20/584
Inventor 张小强施波徐开亮
Owner 和德化学(苏州)有限公司
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