(1) Synthesis of UV-360: Add 323g of UV-329, 4g of powdered sodium hydroxide, 128g of bis(di-n-propylamino)methane and 15g of four Butylammonium bromide was heated to 130°C with stirring, and reacted at this temperature and under vacuum (100mmHg) for 2h, while distilling off the generated di-n-propylamine. Turn off the heat and remove the negative pressure. During the reaction process, 108g of di-n-propylamine (122g in theoretical amount) was recovered, the recovery rate was 88.5%, and the content was 98.6%.
(2) Purification of UV-360: When the temperature drops to 110°C, slowly add 500g of toluene to dissolve all the materials. After the material is dissolved, lower the temperature to 90° C., slowly add 18% hydrochloric acid (about 40 g) by mass, and stir to fully neutralize the material to neutrality. Transfer the reactant to a beaker, cool and crystallize with ice water for 4 to 5 hours, then filter, wash the filter cake twice with 150mL×2 deionized water, then wash twice with 250g×2 methanol, and dry it at 100~ Dry at 110°C to obtain 266g of UV-360 (theoretical yield is 329g), the melting point of the product is 197-198°C, the yield is 80.9%, and the content is 99.6%.
In a 500ml four-neck flask equipped with a stirring thermometer and a condenser, add 100ml of mesitylene, 8.0g of UV-32910, 28.0g of diethylamine, and 7.0g of paraformaldehyde, slowly raise the temperature to 140°C, keep it warm for 1 hour, and distill out the diethylamine at the same time. Ethylamine and water; then add 2.5g of sodium hydroxide, slowly raise the temperature to 170°C, keep the temperature for 2 hours, remove diethylamine and water at the same time, then cool down to 120°C, add glacial acetic acid to acidify to pH5-6, keep stirring for 30 minutes, add 120ml of methanol, heat to reflux, then cool to 10-15°C, keep warm for 60 minutes, filter, and dry the filter cake to obtain Bisoctrizole104.0g, yield 94.5% (in terms of UV-329), liquid chromatograph analysis content 99.77%.
1. Add 0.1 mol of 2-benzotriazole-4-tert-octylphenol, 0.09 mol of paraformaldehyde and 0.18 mol of di-n-propylamine into a four-necked flask, stir and heat, heat up to 120°C after melting the raw materials, and react for 2 hours ;
2. Cool down to 110°C, add 0.4g sodium hydroxide and 35g o-xylene, raise the temperature to 160°C, and react for 10h;
3. Cool down to 110°C, add 7.5g of glacial acetic acid, react for 0.5h, cool down to 60°C, add 40ml of methanol, react for 1h, filter, and recrystallize to obtain Bisoctrizole.
Add 30 grams (1 mole) of formaldehyde and 113 grams (1.5 moles) of N-methylethanolamine into the reaction flask, raise the temperature to 60°C and stir, and after the material liquid is clear and transparent, add 388 grams of dimethyl phthalate ( 2 moles) and 2-(2′-hydroxyl-5′-tertoctylphenyl) benzotriazole 323 grams (1 mole), the temperature was raised to 100 ° C for 2 hours, and then 693 grams of n-chlorotetradecane ( 3 moles) was heated to 160°C for 4 hours. Cool to 90°C, extract with 3 x 100ml of xylene, cool the extract to room temperature, crystallize, filter, and dry the filter cake at 100°C to obtain 270g of light yellow crystalline product with a yield of 82% and a melting point of 197-199°C.