In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 626-40-4 as follows. name: 3,5-Dibromoaniline
This example is a method for preparing 3,5-dibromo-3-methoxy-4-aminoazobenzene, comprising the following steps:(1) Preparation of diazonium salt: In a 100 mL beaker, 5.0114 g of 3,5-dibromoaniline and 8 mL of 20% hydrochloric acid are added, 0Slowly add 1.5232 g of sodium nitrite aqueous solution to the suspension at 0-5 C. The suspension becomes clear and then urea is added to eliminate theThe amount of nitrous acid, sodium acetate solids was adjusted to pH 5, and the clear liquid was placed in ice water for later use.(2) Preparation of sodium o-methoxyanilinosulfonate: A 50 mL round-bottom flask was filled with 10 mL of water and 2.3553 gAfter dissolving sodium bisulfite and sodium bisulfite, 0.7221 g of paraformaldehyde was added. After the reaction at 60C for 35 minutes, 2.4610 g was added dropwise.O-methoxyaniline, the reaction was stopped after 2 h and a mixture of sodium o-methoxyanilino methanesulfonate was obtained.(3) Preparation of azobenzene compound: After the mixture obtained in step (2) is cooled to room temperature, the mixture is stirred under vigorous stirring.Slowly dropping into the diazonium salt obtained in step (1). At this time, the clarified diazonium salt solution gradually becomes dark red viscous liquid, and the temperature is controlled at 0-5 C.The reaction was completed after 6 h. Add 50 mL of 30% aqueous sodium hydroxide, the dark red viscous liquid becomes yellow turbid liquid, nitrogen gasUnder the protection of 50 C hydrolysis 7 h, after the end of the reaction with hydrochloric acid to adjust the pH value of about 8, the crude product was separated by thin layer chromatography to obtain the dye 3,5-Dibromo-3-methoxy-4-aminoazobenzene, 2.237 g (29% yield).
According to the analysis of related databases, 626-40-4, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Lingnan Normal University; Song Xiumei; Feng Zongcai; (9 pag.)CN105152963; (2017); B;,
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