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Author: Subject: Synthesising methyl orange
Keras
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[*] posted on 11-8-2025 at 05:04
Synthesising methyl orange


Folks,

so I had a couple grams of sulphanilic acid I decided to make methyl orange from. It went quite well (the diazo coupling is easy and high yielding) but I was surprised by the ‘shiny’ appearance of the dye flakes. It looks almost what dragon scales could look like.

Has anyone experience with the synthesis? Is that normal? My sulphanilic acid was slightly grey, and I wonder if that greyish impurity is not responsible for that very unusual lustre.

The thing is really hard to dry. It took a whole day in a vacuum desiccator placed under full sunshine on a summer day to get perfectly dry flakes. Once crushed, it is an elegant orange powder, though.

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[*] posted on 11-8-2025 at 05:49


Quote: Originally posted by Keras  

The thing is really hard to dry. It took a whole day in a vacuum desiccator placed under full sunshine on a summer day to get perfectly dry flakes. Once crushed, it is an elegant orange powder, though.


Try washing with pure and anhydrous diethyl ether and place in dessicator.




Water is dangerous if you don't know how to handle it, elemental fluorine (F₂) on the other hand is pretty tame if you know what you are doing.
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[*] posted on 11-8-2025 at 07:28


Quote: Originally posted by Radiums Lab  

Try washing with pure and anhydrous diethyl ether and place in dessicator.


Good idea. Will do that next time.
Well, I got it really dry, but it ruined like 50 g of calcium chloride in the process :p
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SaccharinSlayer157
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[*] posted on 25-9-2025 at 15:40


I just did the same reaction last week for a class I'm taking, the odd shiny reflectivity of the crystals was really striking to me as well, they totally looked like scales. I don't think it had anything to do with purity though considering we were using reagent grade sulfanilic acid and dimethylamine and all my spectra came back pretty clean. Wish I could've kept some :P
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[*] posted on 25-9-2025 at 21:52


Quote: Originally posted by SaccharinSlayer157  
I just did the same reaction last week for a class I'm taking, the odd shiny reflectivity of the crystals was really striking to me as well, they totally looked like scales. I don't think it had anything to do with purity though considering we were using reagent grade sulfanilic acid and dimethylamine and all my spectra came back pretty clean. Wish I could've kept some :P


Lol. Thanks! Nice to have someone with good equipment back me up! :)
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