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Author: Subject: How to synthesise Sulfosalicylic acid
vibbzlab
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[*] posted on 6-11-2019 at 22:24
How to synthesise Sulfosalicylic acid


Do anyone have a procedure for synthesis of sulfosalicylic acid?
I was planning of protein analysis and I need that reagent. I already have the salicylic acid. I was wondering if adding concentrated Sulfuric acid would help me make it or is there a procedure ? If someone knows please do comment
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VSEPR_VOID
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[*] posted on 7-11-2019 at 12:52


http://www.sciencemadness.org/talk/viewthread.php?tid=24147

Here




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[*] posted on 7-11-2019 at 16:03


I am unable to open any pdf in that link. I tried downloading but it says I can't open file
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[*] posted on 8-11-2019 at 14:15




Attachment: sulfosalicylic acid.pdf (317kB)
This file has been downloaded 54 times




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[*] posted on 8-11-2019 at 22:50


Thanks. I am currently doing the procedure for synthesis of sulfosalicylic acid




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[*] posted on 13-11-2019 at 06:39


I heated the salicylic acid with Sulfuric acid and everything dissolved but after I kept it in boiling water bath for about 30min it became black. Is it normal or did it get charred?

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[*] posted on 13-11-2019 at 08:37


surely some tar has formed, how much tar you'll see when you calculate the yield




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[*] posted on 13-11-2019 at 10:01


I could not get crystals even by cooling it




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[*] posted on 13-11-2019 at 11:06


Did you try to crystallize from cold saturated brine as Hexavalent did in 2013?

I do wonder how he got to his yield... I think he expected it to be the dihydrate (probably right) but turned around the 7 and the 8 in his yield.
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[*] posted on 13-11-2019 at 16:11


Yes I tried it in saturated brine




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[*] posted on 24-11-2019 at 03:48


Man I tried my best but I am getting unsuccessful in that last step of sulfonation. On adding Sulfuric acid and heating the whole thing gets charred




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[*] posted on 24-11-2019 at 04:57


Which recipe are you following?

Sulfonating aspirin or sulfonating salycilic acid is not the same! In the later case the phenol is not protected so it is much more sensitive to oxidation and the ring is more susceptible to sulfonation so concentrated sulfuric acid is probably way too much!

Try to find a proper recipe that matches your starting materials!
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[*] posted on 24-11-2019 at 05:57


@vibbzlab; Some time ago I posted links to the 4 volumes of Welcher "Organic analytical reagent". In volume 2 it describes the preparation of this reagent. If you get a black charr you have simply overheated it.
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[*] posted on 24-11-2019 at 07:28


Can I have that link.where to get it




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[*] posted on 24-11-2019 at 08:51


Hi vibbzlab here it is:

https://archive.org/search.php?query=organic%20analytical%20...

Cut and paste this link into your browser if it is not dynamic
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