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.

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.

Quote: Originally posted by Radiums Lab

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

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

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

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