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ChemicalBook CAS DataBase List UV-329

UV-329 synthesis

5synthesis methods
51656-57-6 Synthesis
2-[(2-Nitrophenyl)azo]-4-(1,1,3,3-tetramethylbutyl)phenol

51656-57-6
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Yield:3147-75-9 96.4%

Reaction Conditions:

with methanol;Aminoiminomethanesulfinic acid;sodium hydroxide in toluene at 50 - 80; for 0.5 h;Reagent/catalyst;Solvent;Temperature;

Steps:

1-4

Add 50mL of toluene into a 2000mL flask, add 45.8g (0.1268mol; 98.3%) of 2-(2’-hydroxy-5’-tert-octylphenyl)-nitrodiazobenzene, raise the temperature to 70°C and stir to dissolve.Then lower the temperature to 50°C and add 500mL of 75% methanol solution, and then add 160mL (30%) of sodium hydroxide solution and stir.The temperature was raised to 65°C, 66.41g (0.615mol) of thiourea dioxide was added to the flask and stirred in batches.After the feeding is completed, react at 80°C for 0.5h, and then add dropwise sulfuric acid with a mass concentration of 15% to neutralize the pH to 6-7.Reduce the temperature to 0°C and vacuum filtration, and rinse the filter cake with 50 mL of isopropanol.Drying under vacuum at 65°C for 4h, 40.72g of white product (GC 97%) is obtained, and the yield is 96.4%.

References:

CN112094242,2020,A Location in patent:Paragraph 0018-0021

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