Lost 80% of Yield During Recrystallization

[GodEmperorOfDune]

So I had 1.2g DMT from Gordotek's method, but still enough yellow impurities I wanted to do a recrystallization. I heated heptane to 170f, then added 15ml to the DMT, decanted. Then 10ml, decanted, then 5ml, decanted. The liquid was beautiful and white, and the only thing left in the beaker was the yellow goo. I covered and cooled to room temperature for 4 hours, then 4 hours in the fridge, then overnight in the freezer.

A good deal of the heptane evaporated (I guess I didn't seal it well enough), but I'd imagine that would help crystallization, not hurt it.

I got some beautiful crystals but was left with only 0.287g! What on earth? Where did the rest go? It can't be the yellow plant crud - I didn't have nearly enough of it.

What's with the clear liquid-looking stuff in the dish? Is that related to my problem? (the dish was fully dried)

 

[ben79]

Either:
1. You never had 1.2g of DMT. The product was wet.
2. There's still a lot of DMT in the yellow goo.

If I had to guess, it's probably #2. Try adding more hot heptane to the goo, then decant a sample of the resulting solution (above the goo) to a test tube, close it and put in the freezer.

My bet is that you'll see crystals forms.

Also, it's a good idea to measure the mass of the product (crude or otherwise) every 1 hour so. If the mass goes down - it's still wet. When it stops going down - it's dry.

 

[Sakkadelic]

What ben79 said, but also what exactly do you mean by adding heptane and decanting? You should give it a moment and agitate it to get it to dissolve. Your total of 30 ml heptane can roughly dissolve 1g of dmt at room temp so maybe you needed some more. It's better to use room temp heptane and give it time to dissolve if you want to get a cleaner looking product.

The yellow goo and clear film on the dish is mostly dmt. The droplets look like water condensation but is that on the outside of the dish?