PIPES synthesis

Yield:5625-37-6 86.3%

Reaction Conditions:

with sodium hydroxide in water; pH=9 - 9.5; for 3 h;

Steps:

3; 5; 6 Comparative Example 3:

A preparation method of piperazine ethanesulfonic acid derivative includes the following steps: 1) Mix 44.7g (0.52mol) anhydrous piperazine, 184.5g (1mol) sodium 2-chloroethylsulfonate with 300mL of water, stir evenly, warm to boiling, add 30wt% NaOH solution dropwise to control the pH to 9-9.5, reflux reaction for 3h;2) The reaction solution was cooled to room temperature, concentrated hydrochloric acid was added to the reaction solution to adjust the pH to 1-2, a large amount of white solid was precipitated, filtered, dried and titrated, and the content was 86%;3) Add the solid obtained in step 2) to 600 mL of water, add alkali to dissolve it, filter, collect the filtrate, adjust the pH to 1-2 by adding concentrated hydrochloric acid to the mother liquor, precipitate a large amount of white solid, filter, rinse and pump with absolute ethanol Drying and drying to obtain 134g of light yellow viscous solidified body, the content after titration was 97.2%, and the yield was 86.3%.

References:

CN110683995,2020,A Location in patent:Paragraph 0088-0104