N-Tris(hydroxymethyl)methyl-2-aminoethanesulfonic Acid synthesis
- Product Name:N-Tris(hydroxymethyl)methyl-2-aminoethanesulfonic Acid
- CAS Number:7365-44-8
- Molecular formula:C6H15NO6S
- Molecular Weight:229.25
Yield:7365-44-8 87%
Reaction Conditions:
Stage #1: 1-Bromo-2-chloroethane;2-amino-2-hydroxymethyl-1,3-propanediolwith sodium hydroxide in water; pH=< 7.0; for 4 h;Reflux;
Stage #2: with copper;sodium sulfite in water; for 16 h;Reflux;
Steps:
1-2 Example 1
In 400mL of water, add 143.4g (1mol) of 2-chloro-1-bromoethane and 127.5g (1.05mol) of tris(hydroxymethylaminomethane), and heat to reflux with stirring. During the reaction, the pH value of the reaction was monitored, and the pH value of the reaction solution was controlled to not be lower than 7.0 by adding NaOH aqueous solution (6.0M) dropwise. After refluxing for 4 hours, Add 200mL of water, then add 190g of sodium sulfite and 5g of copper powder catalyst, reflux for 16h, Then the temperature is lowered, the catalyst and insoluble impurities are filtered, and then the cation exchange resin is added, adsorbed, and then separated by filtration to obtain the mother liquor, and then undergo decompression desolvation to remove the solvent. A viscous liquid was obtained. Finally, 400 mL of ethanol was added while it was hot, stirred and dispersed for 1 hour, and filtered to obtain 199 g of white solid. That is, 2-[[tris(hydroxymethyl)methyl]amino]ethanesulfonic acid, the yield of which is about 87%, and the purity of chromatographic analysis is 99%.
References:
CN112479937,2021,A Location in patent:Paragraph 0035-0038
