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Preparation method for 4-tertiary butyl-4'-methoxy dibenzoyl methane

A technology of methoxydibenzoylmethane and methyl tert-butyl benzoate is applied in the field of preparation of 4-tert-butyl-4'-methoxydibenzoylmethane, and can solve the problems of single hetero, large, Problems such as low reaction yield, to achieve the effect of less impurities, high molar yield and less by-products

Active Publication Date: 2012-11-21
HUANGGANG MEIFENG CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of this invention is to provide a preparation method of 4-tert-butyl-4'-methoxydibenzoylmethane, which solves the problems of low reaction yield and large single compound in the past, so that the reaction conversion rate is obviously improved, and the reaction The generated impurities are reduced, which increases the yield, and then through pickling and secondary refining, the product quality is improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Put 30g of p-methoxyacetophenone and 50ml of xylene into a 100ml beaker, stir with a glass rod to dissolve, then transfer to the dropping funnel for later use.

[0019] Add 55g of methyl p-tert-butylbenzoate and 200ml of xylene into a 500ml three-neck flask equipped with mechanical stirring, then add 25g of sodium methoxide, and heat up to 40°C. Add p-methoxyacetophenone solution dropwise. After the dropwise addition, the dropwise addition temperature does not exceed 80°C and keep the temperature for 8 hours, then add hydrochloric acid dropwise, so that the temperature does not exceed 100°C until the pH is less than or equal to 5, and the water layer is separated, and the organic After the layer was washed twice with water, the solvent was removed by distillation under reduced pressure. The solvent can be recycled and used mechanically. Then add 250ml of methanol to obtain the crude product for the first refinement. The crude product is refined for the second time with 2...

Embodiment 2

[0021] Put 30g of p-methoxyacetophenone and 50ml of xylene recovered into a 100ml beaker, stir and dissolve with a glass rod, then transfer to the dropping funnel for subsequent use.

[0022] Add 55g of methyl p-tert-butylbenzoate and 200ml of recovered xylene into a 500ml three-necked flask equipped with mechanical stirring, then add 30g of sodium methoxide, and heat up to 40°C. Add p-methoxyacetophenone solution dropwise. After the dropwise addition, the dropping temperature should not exceed 80°C and keep the temperature for 8 hours. After the layer was washed twice with water, the solvent was removed by distillation under reduced pressure. The solvent can be used mechanically, and then 250ml of the second refining mother liquor is added. Batches of crude product were refined, filtered and dried to obtain 55.5 g of off-white product. The content is ≥99%, and the product molar yield based on p-methoxyacetophenone is 86.7%.

Embodiment 3

[0024] Put 30g of p-methoxyacetophenone and 50ml of xylene recovered into a 100ml beaker, stir and dissolve with a glass rod, then transfer to the dropping funnel for subsequent use.

[0025] Add 45g of methyl p-tert-butylbenzoate and 200ml of recovered xylene into a 500ml three-neck flask equipped with mechanical stirring, then add 30g of sodium ethoxide, and heat up to 40°C. Add p-methoxyacetophenone solution dropwise. After the dropwise addition, the dropping temperature should not exceed 80°C and keep the temperature for 8 hours. After the layer was washed twice with water, the solvent was removed by distillation under reduced pressure. The solvent can be recycled and used mechanically. Then, 250ml of methanol was added to obtain the crude product for the first refinement. The crude product was refined for the second time with 250ml of methanol. The crude product was refined, and 55g of off-white product was obtained after suction filtration and drying. The content is ≥99...

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Abstract

The invention relates to a preparation method for 4- tertiary butyl-4'-methoxy dibenzoyl methane, which belongs to the technical field of fine chemical engineering. The preparation method for the 4-tertiary butyl-4'-methoxy dibenzoyl methane comprises the following steps of: (1) evenly mixing p methoxy acetophenone with solvent; (2) evenly mixing p-tert-butylbenzoic acid methyl ester with the solvent, adding sodium methoxide or sodium ethylate accounting for 60-100wt% of the p methoxy acetophenone, heating to 40-100DEG C, dropwise adding the p methoxy acetophenone solution, finishing dropwise adding until the mass ratio of the p methoxy acetophenone to the p-tert-butylbenzoic acid methyl ester is 0.6-2.0, and continuing to carry out insulation reaction; (3) after reaction is complete, obtaining a crude product, regulating the pH (potential of hydrogen) of the obtained crude product to be less than or equal to 5, carrying out dissolved clarification after stirring, washing with water, and layering; and (4) after solvent is removed from the material washed with water, adding methyl alcohol to dissolve, decoloring by activated carbon, repeatedly adding the methyl alcohol, and refining again to obtain the product. The preparation method for the 4-tertiary butyl-4'-methoxy dibenzoyl methane has the advantages of high molar yield and moderate reaction condition and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of 4-tert-butyl-4'-methoxydibenzoylmethane, which belongs to the technical field of fine chemicals. Background technique [0002] 4-tert-butyl-4'-methoxydibenzoylmethane, also known as Bassoon 1789, chemical formula C 20 h 22 o 3 , molecular weight 310.39, white crystalline powder, is a kind of spectrum oil-soluble UVA ultraviolet absorber. It has a strong absorption effect on ultraviolet rays (320-400nm) in the A area, and the ultraviolet A area is defined as the "tanning area", so the current whitening cosmetics are added with 4-tert-butyl-4'-methoxydiphenyl Formylmethane. It is mainly used in sunscreen products such as sunscreen and sunscreen lotion, and can also be used as a stabilizer to prevent the photodecomposition of cosmetics and perfumes. The main application is UV absorber, sunscreen agent, and its O / W mild anionic emulsifier / stabilizer, easy to operate and shape. Suitable for PH3~9 range ...

Claims

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Application Information

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IPC IPC(8): C07C49/84C07C45/72
Inventor 李小林陈军辉徐文立
Owner HUANGGANG MEIFENG CHEM TECH
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