A kind of preparation method of ultraviolet absorber etocrine
A technology based on Lilin and absorbents, applied in the field of preparation of ultraviolet absorbents, can solve the problems of high toxicity of benzene, unsuitability for industrial production, difficult treatment of waste acetic acid containing water, etc., achieve low production cost, short reaction time, and avoid solvents The effect of loss
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Embodiment 1
[0030] Put 364g (2.0mol) of benzophenone, 452g (4.0mol) of ethyl cyanoacetate, 44g (0.3mol) of glutamic acid and 7.5g (0.1mol) of glycine into a 1L reaction flask, and raise the temperature to 50°C to observe the reaction Start stirring after the solid in the bottle is basically dissolved, and bring a vacuum. Continue to raise the temperature to about 80°C, and water will continue to distill out. During the reaction, gradually increase the reaction temperature to 95-100°C, and stop the reaction until no water appears in the condenser. The reaction time is 16-18 hours.
[0031] Transfer all the materials in the reaction bottle into a 2L reaction bottle, add 460g of water, and stir at 60-70°C for 30 minutes, then pour into a separatory funnel while hot to separate layers to obtain 782g of oil layer and 503g of water layer. The water layer was distilled under reduced pressure, and the water was distilled at 50-100°C until solids appeared (a total of 382g of water was distilled ou...
Embodiment 2
[0035] Put 330g benzophenone, 230g ethyl cyanoacetate, 222.6g reclaimed ethyl cyanoacetate, 42.8g reclaimed etorylene and benzophenone mixture, 63.6g reclaimed aqueous catalyst into a 1L reaction flask, and add 4.5g of fresh glutamic acid and 0.8g of glycine were heated up to 50°C to observe that the solids in the reaction flask were basically dissolved, and then began to stir, and put on a vacuum. Continue to raise the temperature to about 80°C, and water will continue to distill out. During the reaction, the reaction temperature is gradually increased to 95-100°C, and the reaction ends when no water appears in the condenser. The reaction takes 18-20 hours.
[0036] Transfer all the materials in the reaction bottle into a 2L reaction bottle, add 382g of distilled and recovered water and 78g of fresh water, and stir at 60-70°C for 30 minutes, pour into a separatory funnel while hot and separate to obtain 802g of oil layer, water Layer 512g. The water layer is distilled under...
Embodiment 3
[0040]Put 364g (2.0mol) of benzophenone, 452g (4.0mol) of ethyl cyanoacetate, 40g (0.3mol) of aspartic acid and 11.5g (0.1mol) of proline into a 1L reaction flask and raise the temperature to 50 ℃ observed that the solid in the reaction bottle was basically dissolved and started to stir, and put on a vacuum. Continue to raise the temperature to about 80°C, and water will continue to distill out. During the reaction, the reaction temperature is gradually increased to 95-100°C, and the reaction ends when no water appears in the condenser. The reaction takes 18-19 hours.
[0041] Transfer all the materials in the reaction bottle into a 2L reaction bottle, add 580g of water, and stir at 60-70°C for 30 minutes, then pour into a separatory funnel while hot to separate layers to obtain 791g of oil layer and 615g of water layer. The water layer was distilled under reduced pressure, and the water was distilled at 50-100°C until solids appeared (a total of 502g of water was distilled o...
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