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Synthetic method of 2-hydroxy-4-methoxybenzophenone

A technology of methoxybenzophenone and synthesis method, which is applied to the preparation of carbon-based compounds, chemical instruments and methods, and condensation to prepare carbonyl compounds, etc., which can solve problems such as low product yield, low product purity, and complex production process , to achieve the effect of simple reaction process, full and complete reaction, and easy operation

Inactive Publication Date: 2014-11-26
江苏德峰药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the traditional process of 2-hydroxy-4-methoxybenzophenone uses resorcinol, benzoyl chloride, chlorobenzene, etc. as raw materials, and is synthesized through traditional methylation, Friedel-Crafts, hydrolysis and other reactions. , the production process is complicated, the product purity is low, and the product yield is only 50-55%. Now, 2,4-dihydroxybenzophenone and dimethyl sulfate are used as raw materials to directly synthesize 2-hydroxy-4-methoxy base benzophenone, but the prior art production process is complicated, the product purity is low, and the phenomenon that the product yield is low still exists

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0020] Condensation reaction: Add 180ml of solvent methanol and 66g of resorcinol to a 500ml three-necked flask. After heating up and dissolving, add 6g of catalyst zinc chloride, then raise the temperature to 45°C, start adding 135g of trichlorotoluene dropwise, and control the temperature not to exceed 55°C. ℃, drop over 1h. After controlling the temperature at 55-60°C for 6 hours, raise the temperature to 70°C for 1 hour, cool to below 20°C, and filter. Wash with hot water at 50-60°C until neutral. Dry at 80°C for 6 hours, and the obtained product is 124g.

[0021] Methylation reaction: In a 250ml three-necked flask, add 8.2g of sodium hydroxide, dissolve in 100ml of water, and cool down to 5°C. Add 42.8g of 2,4-dihydroxybenzophenone, then lower the temperature to below 0°C, start to drop 30.6g of dimethyl sulfate, and control the dropping time for 1h. After the dropwise addition was completed, the temperature was controlled at 0-2°C and the reaction was stirred for more...

Embodiment 2

[0024] Condensation reaction: Add 170ml of solvent ethanol and 55g of resorcinol to a 500ml three-necked flask. After heating up and dissolving, add 2.7g of catalyst zinc chloride, then raise the temperature to 50°C, start to add 102.6g of trichlorotoluene dropwise, and control the temperature. More than 55 ℃, 1h dripping. After controlling the temperature at 55-70°C for 6 hours, raise the temperature to 75°C for 1 hour, cool to below 20°C, and filter. Wash with hot water at 50-60°C until neutral. Dry at 80°C for 6 hours, and the obtained product is 125g.

[0025] Methylation reaction: In a 250ml three-necked flask, add 4.1g of sodium hydroxide, dissolve in 54ml of water, and cool down to 5°C. Add 21.4g of 2,4-dihydroxybenzophenone, then lower the temperature to below 0°C, start to drop 10.8g of dimethyl carbonate, and control the dropping time for 1h. After the dropwise addition, control the temperature at 0-2°C and stir the reaction for more than 6 hours, remove the solve...

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Abstract

The invention discloses a synthetic method of 2-hydroxy-4-methoxybenzophenone. The method comprises the following steps: condensing main raw materials comprising benzenyltrichloride and resorcinol, methylating, and purifying to obtain a final product. Compared with traditional synthetic methods, the synthetic method of 2-hydroxy-4-methoxybenzophenone has the advantages of reduction of Friedel-Crafts and hydrolysis reaction steps through primarily carrying out condensation, simple reaction technology and easy operation; the set of a feed ratio makes the reaction full and complete, so a largest yield is guaranteed; and the final product is obtained through filtering, re-crystallizing and purifying, the purity of the product can reach 95-98%, and the yield of the product can reach above 90%.

Description

technical field [0001] The invention relates to a synthesis method of 2-hydroxy-4-methoxybenzophenone, which belongs to the field of chemical synthesis. Background technique [0002] 2-Hydroxy-4-methoxybenzophenone is used in plastics, chemical fibers, paints and petroleum products, especially for light-colored transparent products. It can be used in paints and various plastic products. It is suitable for polyvinyl chloride, polyester, Acrylic, resin, polystyrene and light-colored transparent furniture are especially effective, and it is a good cosmetic additive. Benzophenone UV absorber is an excellent stabilizer for polyethylene and other synthetic plastics. The dosage is 0.5-1.5%. It can also be used in paint, pigment, coating industry, refined paraffin and daily cosmetics. It is a broad-spectrum ultraviolet absorber, which has the advantages of high absorption rate, non-toxicity, non-teratogenic effect, good light and thermal stability, etc. It can absorb UV-A and UV-B ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/61C07C49/84C07C45/45C07C49/83
CPCC07C45/64C07C45/008C07C45/45C07C49/84C07C49/83
Inventor 王德峰石飞俞健钧
Owner 江苏德峰药业有限公司
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