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The preparation method of 2,2'-dihydroxy-4-methoxybenzophenone

A technology of methoxybenzophenone and trihydroxybenzophenone, which is applied in the field of chemical synthesis, can solve the problems of low preparation yield, undisclosed preparation method for product purification, and high cost, so as to improve the preparation efficiency and solve the problem of product Effects of appearance problems, yield and quality improvement

Active Publication Date: 2017-07-14
宜都市华阳化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The starting material salicyloyl chloride of the preparation method has poor stability, high cost, and low preparation yield. The literature does not disclose the preparation method for the purification of the product, and the process scheme is not suitable for industrial production.

Method used

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  • The preparation method of 2,2'-dihydroxy-4-methoxybenzophenone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 50g sulfolane, 20mL phosphorus oxychloride, 30g (0.2mol) anhydrous zinc chloride in a 250mL four-neck glass bottle, stir and heat to 50°C for 1 hour, then add 15.2g (0.11mol) of salicylic acid, Resorcinol 11.0g (0.1mol) was heated to 75°C and reacted for 2 hours. After the reaction was completed, 20mL of water was added dropwise under cooling to terminate the reaction. 21.3g, the content of 2,2',4-trihydroxybenzophenone detected by HPLC was 96.58%, and the yield was 92.60%;

[0028] Take 21.3g of the prepared 2,2',4-trihydroxybenzophenone in a 250mL reaction flask, add 60mL of toluene, 12.7g (0.12mol) of sodium carbonate, stir and heat up to 45°C, add dropwise dimethyl sulfate 16.4 g (0.13 mol) was added and kept for 2 hours after dripping, washed with 50 mL of distilled water, and after stirring for 10 minutes, the water was separated, the organic phase was distilled at 140° C. to distill out toluene, and then 19.97 g of the BP-8 crude product mixture was distill...

Embodiment 2

[0031] Weigh 250g of sulfolane, 100mL of phosphorus oxychloride, 150g (0.2mol) of anhydrous zinc chloride, add them to a 1000mL reaction flask with stirring, heat to 55°C for 1 hour, and then add 72.5g (0.53mol) of salicylic acid , Resorcinol 55.0g (0.5mol), heated to 72 ℃ and reacted for 2 hours, after the reaction was completed, 50mL of water was added dropwise under cooling to terminate the reaction, the reaction solution was poured into 1000mL of ice water and stirred for 10 hours, crystallized by cooling, after filtration at room temperature The product was collected, weighed 108.3 g after drying, GC detected 2,2',4-trihydroxybenzophenone content of 95.20%, and the yield was 94.17%;

[0032] Take 108.3g of the prepared 2,2',4-trihydroxybenzophenone in a 1000mL reaction flask, add 300mL of toluene, 63.5g (0.60mol) of sodium carbonate, stir and heat up to 45°C, add dropwise dimethyl sulfate 82.0 g (0.65 mol) was added and kept for 2 hours after dropping, washed with 250 mL ...

Embodiment 3

[0035] Take by weighing 500kg sulfolane, 200L phosphorus oxychloride, 300kg (2000mol) anhydrous zinc chloride, add in 1000L enamel reaction tank, be warming up to 50 ℃ of reaction 1 hour, then add salicylic acid 152kg (1100mol), resorcinol 110kg (1000mol), heating controlled 70-75 ℃ of reaction for 2 hours, after the reaction finished, drip 100L of water to stop the reaction, the reaction solution was transferred into the 2000L enamel reaction tank that had been cooled and housed with 1000L of ice water and stirred for 8 hours, crystallized by cooling, and centrifuged, After drying, the weight is 208kg, the content of 2,2',4-trihydroxybenzophenone detected by HPLC is 97.15%, and the yield is 90.43%;

[0036] Get prepared 2,2', 208kg (904mol) of 4-trihydroxybenzophenone in 2000L enamel reaction tank, add about 600kg toluene, 127kg (1200mol) sodium carbonate, stir and be warming up to 45 ℃, drip sulfuric acid two 164kg (1300mol) of methyl ester, dripped and incubated for 2 hours...

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Abstract

A preparation method of 2,2'-dihydroxy-4-methoxybenzophenone comprises the following steps: synthesizing 2,2'4-trihydroxybenzophenone from salicylic acid and resorcinol, and carrying out a methylation reaction on 2,2'4-trihydroxybenzophenone and dimethyl sulfate to prepare 2,2'-dihydroxy-4-methoxybenzophenone. The method has the advantages of high purification efficiency, good separation effect of byproducts, high product purity reaching 99.5%, and realization of industrial production requirements of the above product.

Description

technical field [0001] The invention belongs to the field of chemical synthesis and relates to the preparation of a light stabilizer, in particular to a preparation method of 2,2'-dihydroxy-4-methoxybenzophenone, a benzophenone type ultraviolet absorber. Background technique [0002] 2,2'-Dihydroxy-4-methoxybenzophenone, hereinafter referred to as BP-8, is a kind of ultraviolet absorber. The ultraviolet light of 330-370nm has a strong absorption effect and has a wide absorption range. It is suitable for polymer materials PVC, ABS resin, acrylic resin, polyurethane, melamine resin, cellulose resin and cosmetics. [0003] There are few literature reports on the preparation method of BP-8. The following is the relevant literature on the synthesis method of BP-8. [0004] In the "Synthesis of 2,2'-dihydroxy-4-methoxybenzophenone" published by Liu Shumei et al. 2,2'-dihydroxy-4-methoxy benzophenone was selectively removed from two methyl groups to form 2,2'-dihydroxy-4-methox...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/70C07C49/84
CPCC07C45/455C07C45/70C07C49/84C07C49/83
Inventor 徐明华赵定春覃华中
Owner 宜都市华阳化工有限责任公司
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