1,4-Butane-disulfonate synthesis

Yield:-

Reaction Conditions:

with hydrogenchloride in methanol;water at 40 - 50;Solvent;

Steps:

3.1 synthesis of 1,4-butanedisulfonic acid
To the reaction flask was added 285 g (1.09 mol) of sodium 1,4-butanedisulfonate,900 g of anhydrous methanol,Hydrogen chloride gas prepared by the dry purification system into the reaction bottle,Temperature control in the 40 ~ 50 ° C,Acidification to the reaction solution of hydrogen chloride content> 10wt% when the acidification reaction is completed,And concentrated under reduced pressure.With a number of vacuum distillation of anhydrous methanol to bring out hydrogen chloride,And then high vacuum concentration to bring out hydrogen chloride. 500 g of glacial acetic acid was added,crystallization,filter,dry,A white crystal 1,4-butanedisulfonic acid crude 215g. Yield 90.8%HPLC content> 90%.

References:

Henan yu Chen pharmaceutical co., LTD;LU, MING;GUO, XUECHAO;WEI, LIQIANG;LIU, SHUGANG;YE, JIDONG;LIU, YUCENG CN104086463, 2016, B Location in patent:Paragraph 0030; 0031; 0032

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