Novel process for preparing sun-screening agent 2-hydroxy-4-n-octyloxy benzophenone

A technology of n-octyloxybenzophenone and dihydroxybenzophenone, which is applied in the preparation of carbon-based compounds, organic compounds, organic chemistry, etc., to reduce the generation of waste water and residue, easy to control the intermediate reaction process, The effect of reducing the three wastes

Pending Publication Date: 2021-02-05
马鞍山科思化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method not only reduces the cost of raw materials, but also solves the current problem of industrial waste water. In addition, the whole process has mild conditions, less waste, high yield, good product quality, and meets the requirements of the cosmetics industry. The process is simple to operate and easy to implement. The intermediate reaction process is simple and easy to control, and industrialized production can be realized, thereby completing the present invention

Method used

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  • Novel process for preparing sun-screening agent 2-hydroxy-4-n-octyloxy benzophenone
  • Novel process for preparing sun-screening agent 2-hydroxy-4-n-octyloxy benzophenone
  • Novel process for preparing sun-screening agent 2-hydroxy-4-n-octyloxy benzophenone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0093] Preparation of 2,4-dihydroxybenzophenone

[0094] Add 660.6g of 10% ethanol-water solution and 110.1g of resorcinol into a 2000mL four-necked glass reaction flask equipped with a stirrer, thermometer, dropping funnel and condenser, and start stirring.

[0095] The system was heated to 60°C, and 234.6 g of trichloromethylbenzene was slowly added dropwise within 2 hours. After the dropwise addition, the reaction was continued at 80°C for 6 hours.

[0096] Add toluene for extraction, and the oil layer is 2,4-dihydroxybenzophenone required for the preparation of 2-hydroxy-4-n-octyloxybenzophenone.

Embodiment 2

[0098] Preparation of 2-hydroxy-4-n-octyloxybenzophenone

[0099] In a 1000mL four-necked glass reaction flask, add 1200g of toluene, 400g of 2,4-dihydroxybenzophenone, 330g of 1-chloro-n-octane, and 120g of potassium carbonate in sequence, in which 2,4-dihydroxybenzophenone is Embodiment 1 gains.

[0100] Heat the temperature to 80°C, keep it warm for 6 hours until the reaction of the raw materials is complete, raise the temperature to 110°C, adjust the pressure to -0.1MPa for precipitation, then raise the temperature to 220°C, adjust the pressure to 1mmHg for distillation, and finally add ethanol to recrystallize to obtain 2-Hydroxy-4-n-octyloxybenzophenone, yield 90%.

Embodiment 3

[0102] Preparation of 2-hydroxy-4-n-octyloxybenzophenone

[0103] In a 1000mL four-necked glass reaction flask, add 1200g of N-N dimethylformamide, 400g of 2,4-dihydroxybenzophenone, 330g of 1-chloro-n-octane, and 120g of catalyst sodium carbonate in sequence.

[0104] Heat the temperature to 70°C, keep it warm for 8 hours, until the raw materials are completely reacted, raise the temperature to 120°C, adjust the pressure to -0.1MPa for precipitation, then raise the temperature to 230°C, adjust the pressure to 1mmHg for distillation, and finally add ethanol for recrystallization 2-Hydroxy-4-n-octyloxybenzophenone was obtained with a yield of 95%.

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Abstract

The invention discloses a novel process for preparing a sun-screening agent 2-hydroxy-4-n-octyloxy benzophenone. According to the process, 2,4-dihydroxy benzophenone is prepared, and 2,4-dihydroxy benzophenone and 1-chloro-n-octane are used as raw materials, wherein the prepared 2,4-dihydroxy benzophenone is simple in method, has no need of posttreatment and can be directly used as a reaction rawmaterial for subsequent reaction, and the energy consumption is reduced from the source; 1-chloro-n-octane is taken as an alkylation reagent, inorganic base is taken as a catalyst, solvents are addedfor reaction, and the yield of the obtained product 2-hydroxy-4-octyloxybenzophenone is high and can reach 90% or above. According to the method, the raw material cost is reduced, the problem of industrial wastewater at present is solved, in addition, the whole process is mild in condition, few in three wastes, high in yield and good in product quality, the use requirements of the cosmetic industry are met, the technological process is simple to operate and easy to realize, the intermediate reaction process is simple and easy to control, and industrial production can be realized.

Description

technical field [0001] The invention belongs to the field of chemical technology, and in particular relates to a technology of sunscreen agent 2-hydroxy-4-n-octyloxybenzophenone. Background technique [0002] Because the sun's rays contain a large amount of ultraviolet light harmful to colored objects, with a wavelength of about 290-460 nanometers, these harmful ultraviolet light will eventually decompose and fade the color molecules through chemical oxidation and reduction, and use sunscreen to protect the protected objects. Objects and human skin can effectively prevent or weaken its damage to color. Sunscreen is a light stabilizer that can absorb ultraviolet rays from sunlight and fluorescent light sources without changing itself. [0003] 2-Hydroxy-4-n-octyloxybenzophenone (alias: ultraviolet absorber UV-531) is a kind of sunscreen agent, and its molecular formula is C 21 h 26 o 3 , melting point is 47-49°C, color is light yellow or white crystalline powder, can stro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/84C07C45/64
CPCC07C45/64C07C45/008C07C49/84C07C49/825
Inventor 王宁宁廉云刘一杰王剑秋
Owner 马鞍山科思化学有限公司
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