With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.103-76-4,N-(2-Hydroxyethyl)piperazine,as a common compound, the synthetic route is as follows.
The preparation method of 4-hydroxyethylpiperazine ethanesulfonic acid includes the following steps: 1) Mix 260g (2mol) 2-hydroxyethylpiperazine, 165g (0.94mol) sodium 2-chloroethylsulfonate with 120mL water, stir well, the reaction solution becomes clear, the pH is about 10,Heat up to 85 , stop heating until the system self-heats to 103-105 ,The reaction is heated to reflux for 30min, the reaction is over, and the pH is about 8;2) Cool the reaction liquid to 60 C, add triethylamine to the reaction liquid to adjust the pH to 7-8, 1.5 L of absolute ethanol and 8 g of activated carbon, boil for 30 min, and filter while hot;3) Adjust the pH of the filtrate to 5 using glacial acetic acid, stir the filtrate and cool to 5 C to crystallize overnight,Filter and dry to obtain 310g of crude product, which is 95% by drying after titration inspection; 4) Dissolve the sample obtained in step 3) in 750 mL of ethanol and heat to reflux, Add 145mL of water, stir to dissolve, filter while hot, and the filtrate is cooled to 5 overnight, Filtration gave 181g of 4-hydroxyethylpiperazineethanesulfonic acid crystals, After drying, 175g of 4-hydroxyethylpiperazineethanesulfonic acid was obtained, and the content was 99.8% after titration; 5) Concentrate the mother liquor under reduced pressure to a volume of 30-40%, add activated carbon to boil for decolorization, filter while hot, the filtrate is cooled to 0-5 C, filtered, dried and recovered to obtain 15g of 4-hydroxyethylpiperazineethanesulfonic acid After titration, the content was 99.6%, and the total yield was 84.7%., 103-76-4
As the paragraph descriping shows that 103-76-4 is playing an increasingly important role.
Reference£º
Patent; Suzhou Yake Technology Co., Ltd.; Yuan Yongkun; (10 pag.)CN110683995; (2020); A;,
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