Extraction help - mixed solvent mishap

[84pa11]

I messed up and pretty sure I performed an extraction with a mixture of heptane and acetone. Dumb mistake, but had a mislabeled jar that I thought was old heptane (but believe now was actually used acetone from the freebase to fumerate conversion). During th extraction I used this jar plus some new heptane, hence the mixture of heptane and acetone.

I just pulled off this solution and placed it in the freezer. Waiting to see what I have tomorrow. Worried the dmt might not crystalized since it could just dissolve into the acetone straight away. Anyone screw up like this before . Dumb mistake I know, I'll be more careful in the future.

If it doesn't crystalize, one idea I have is to boil off the acetone since it has a lower boiling point than the heptane (will be very careful when doing this, and in a well ventilated area). But welcome any thoughts or other ideas.

 

[Transform]

I messed up and pretty sure I performed an extraction with a mixture of heptane and acetone. Dumb mistake, but had a mislabeled jar that I thought was old heptane (but believe now was actually used acetone from the freebase to fumerate conversion). During th extraction I used this jar plus some new heptane, hence the mixture of heptane and acetone.

I just pulled off this solution and placed it in the freezer. Waiting to see what I have tomorrow. Worried the dmt might not crystalized since it could just dissolve into the acetone straight away. Anyone screw up like this before . Dumb mistake I know, I'll be more careful in the future.

If it doesn't crystalize, one idea I have is to boil off the acetone since it has a lower boiling point than the heptane (will be very careful when doing this, and in a well ventilated area). But welcome any thoughts or other ideas.

Yes, the acetone will inhibit freeze precipitation entirely. I made a similar mistake once, except it was with IPA in naphtha.

You might as well take it out of the freezer now. Evaporation is one option, although selective removal of the acetone would require fractional distillation and both the associated apparatus and skillset.

If, instead, you wash the DMT and the acetone out of the heptane with some diluted vinegar you can then boil the acetone out of the water and either evaporate it all down to retrieve DMT acetate salt as a waxy solid or - if for some reason you van't get distilled water, for example, redsce the acidic washes down to a manageable volume before adding sodium hydroxide solution.

When you've cleaned up the heptane satisfactorily - giving it one more wash with sodium carbonate solution for good luck, and maybe even a prior wash with sodium bisulfite solution - you should be able to reuse it for pulling the DMT back out of the washes and freeze precipitating as before.

Separation of Aldehydes and Reactive Ketones from Mixtures Using a Bisulfite Extraction Protocol - PMC

The purification of organic compounds is an essential component of routine synthetic operations. The ability to remove contaminants into an aqueous layer by generating a charged structure provides an opportunity to use extraction as a simple ...

pmc.ncbi.nlm.nih.gov