Method for synthesizing arbutin using solid superacid as catalyst
A solid superacid and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve problems such as poor reaction selectivity, low yield, and a large amount of waste acid
Active Publication Date: 2022-07-05
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
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[0034] A method for synthesizing arbutin using solid superacid as catalyst, which comprises the steps:
[0035]S1, the preparation of solid super acid catalyst: Dissolve 20g FeCl3 in 200g deionized water, add 100g ammonia precipitant, precipitate at room temperature for 12hrs to obtain Fe(OH)3 sol, filter, wash with 20g deionized water, 100- After drying at 120°C, it was lowered to room temperature, impregnated with 100ml of 2.5mol / L sulfuric acid solution, filtered and dried, dried and calcined at 300-500°C for 8-20hrs, and then lowered to room temperature in a dry nitrogen environment to obtain a tan catalyst about 22g;
[0036] S2, the preparation of intermediate Arb-1: 120g of acetic anhydride and 12g of sodium acetate were added to the reaction kettle in turn, the temperature was raised to 60-80°C with stirring, 40g of glucose was added in 3 batches, and the reaction temperature was controlled to be less than or equal to 100°C. The temperature was controlled at 120-125°C...
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In the dehydration reaction of the key intermediate for synthesizing arbutin in the current process route, the dehydrating agent used is boron trifluoride diethyl ether, which belongs to inflammable and explosive articles, and another type of dehydrating agent is sulfuric acid, p-toluenesulfonic acid. Strong acid, when using this type of dehydrating agent, has poor reaction selectivity, low yield, and produces a large amount of waste acid at the same time, which faces great environmental protection pressure. In view of this, the present invention proposes a method for synthesizing arbutin using a solid superacid as a catalyst, which comprises the following steps: preparing a solid superacid catalyst; using the solid superacid as a catalyst to prepare an intermediate Arb-1; Preparation of intermediate Arb-2 from Arb-1 as a catalyst; recovery and activation of the catalyst; reaction and purification of intermediate Arb-2, methanol and sodium methoxide to obtain arbutin, the process has the advantages of less three wastes, green environmental protection , the process operation is simple and convenient, suitable for industrialization and so on.
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 a white needle-like crystal or powder. The leaves extracted from bearberry can inhibit the activity of tyrosinase in the body and prevent the production of melanin, thereby reducing skin pigmentation, removing pigmentation and freckles, and also has bactericidal and anti-inflammatory effects. Mainly used for the preparation of advanced cosmetics. In the dehydration reaction of the key intermediate for synthesizing 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 application. Repeated application, these are unfavorable to adopt this route to carr...
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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