1-(2-Hydroxy-3-sulfopropyl)-pyridinium betane synthesis

Yield:3918-73-8 99.1%

Reaction Conditions:

with sodium metabisulfite;tetrabutylammomium bromide;sodium sulfite in water at 30 - 50; under 18751.9 - 26252.6 Torr;Large scale;Temperature;Pressure;

Steps:

1-4 Example 3

Dissolving 2000 g of sodium metabisulfite in 5450 g of deionized water, after it is completely dissolved,Add 3 g of sodium sulfite and 0.4 g of tetrabutylammonium bromide to the sodium metabisulfite solution.After stirring and mixing uniformly, the mixture containing HSO3- is filtered through a membrane and then introduced into a metering pump.Then the mixture containing HSO3- is at a rate of 90 g/min,1948g of epichlorohydrin was simultaneously introduced into the first microchannel reactor at a rate of 23g/min.Adjusting the reaction temperature in the first microchannel reactor to 30 ° C, adjusting the back pressure valve to stabilize the pressure of the first microchannel reactor at 2.5 MPa,Passing the reaction product in the first microchannel reactor into the second microchannel reactor,Simultaneously, 1665 g of pyridine was introduced into the second microchannel reactor at a feed rate of 22 g/min.And a mixture of 3g 1,4,7,13-tetraoxa-10-aza-2,3-benzocyclopenta-2-ene,The reaction temperature in the second microchannel reactor was adjusted to 50 ° C, and the back pressure valve was adjusted so that the pressure of the second microchannel reactor was 3.5 MPa.The reacted material is directly introduced into a storage tank with a cooling water jacket to obtain a colorless, clear and transparent liquid.The sample was analyzed by HPLC analysis, and the purity of the product obtained by the method of the present example was 99.76%., the yield is 99.1%, the color is 15 (platinum cobalt colorimetric method),The Hull cell test piece passed the test.

References:

CN109265392,2019,A Location in patent:Paragraph 0029-0039