Synthetic Route of 50739-76-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 50739-76-9, name is (2-Amino-3,5-dibromophenyl)methanol, molecular formula is C7H7Br2NO, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
Adding 4.84kg of N-methylcyclohexylamine and 0.44kg of toluene to a 30L glass reactor with a water separator5.0 kg of 3,5-dibromo-2-aminobenzyl alcohol, 0.5 kg of solid super acid SiO2-OSO3H (SSA), 1.2 kg of acetic acid, and then heated to 85 C for a total of 12 hours after stirring.Sampling UPLC test (take the reaction solution as a sample at a concentration of approximately 275 mg/ml).After passing the reaction (3,5-dibromo-2-aminobenzyl alcohol is not more than 5.0%), it is concentrated under reduced pressure until no significant fraction is distilled off, and the residue is transferred to a barrel and cooled to room temperature, and then 12 kg of acetone is added.The solution was then transferred to a 100 L double-layer glass reactor and adjusted to pH 2 – 3 with 15% hydrochloric acid to precipitate a solid. After 20 minutes,Repeat the measurement of pH 2 ~ 3; continue to stir for 1 hour, then continue to cool to 0 C for 4 hours, centrifugal filtration, to obtain bromohexine hydrochloride wet,The wet product is placed in a blast drying oven tray, dried at 35±5C, and turned once every 3 hours.After drying for 10 hours, 6.24 kg was obtained after the water was qualified, and the yield was 85%. Bromohexidine hydrochloride refined: Adding 42.0 kg of 95% ethanol and 6.2 kg of crude bromohexidine hydrochloride to a 100 L enamel reactor.The temperature was raised to reflux, stirred and dissolved, and then 0.15 kg of activated carbon was added, and the mixture was decolorized by stirring for 1 hour.The titanium rod was filtered, and the filtrate was transferred to a 100 L double-layer glass reactor and slowly cooled to room temperature.Then, the crystallized mixture was stirred at room temperature for 2 hours, and then cooled to 5 C and stirred for 5 hours.The mixture was filtered by centrifugation, and the filter cake was rinsed with a small amount of 95% ethanol to obtain bromohexine hydrochloride wet product.The bromohexine hydrochloride wet product is placed in a vacuum drying oven tray and dried at 60 C, and the degree of vacuum is less than -0.08 mPa.The material was turned over once every 2 hours, dried for 12 hours, and the water was qualified to receive 4.96 kg, and the yield was 80%.
According to the analysis of related databases, 50739-76-9, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Guangzhou Yipinhong Pharmaceutical Co., Ltd.; Guangdong Zerui Pharmaceutical Co., Ltd.; Li Hanxiong; Lan Xiaobing; Yan Xinxing; (20 pag.)CN109535010; (2019); A;,
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