Screwed freebase conversion rate and oil?

[NimbleSoda]

Hey all :thumb_up: I'm pretty sure this should be a relatively easy question for you guys...

A friend freebased what was almost 13g of DMT fumarate, and ended up with 4g of DMT freebase goo. He definitely carried out the reaction 100% till there was no more freebase forming.

Does that just mean that probably a lot of that fumarate was like, oils or fats or something? Friend did his extraction with Xylene throughout, and even though he did a defat he assumes there was probably a fair bit of oils toward the end still. Should he do multiple defats next time to get rid of more oils?

He also assumes that the waxy goo he ends up with is mostly cause of NMT, what do you guys think of that? Would it be enough to just do a heptane re-X or will he have to use dry ice to rid the NMT to solidify the end product? Thanks so much for all comments

 

[downwardsfromzero]

It's possible the fumarate may have contained a large amount of sodium fumarate, which would account for the very poor yield from the conversion.

Without further details of both the entire extraction procedure and the conversion process it's not really that meaningful to speculate.

If you're thinking it's something to do with NMT, that kind of implies that ACRB was the plant material used. The comment about defatting implies perhaps an acidic phase was used before base was added; and you state that xylene was used throughout so I'm guessing you used FASW or FASA to get the alkaloids back out of the xylene.
You'll have to say what method was used for converting fumarate to freebase.

That's quite a big extraction you must have done, btw.

 

[NimbleSoda]

Without further details of both the entire extraction procedure and the conversion process it's not really that meaningful to speculate.

Thanks for the reply

12hr acid boils on 500g ACRB > reduced > basify with sodium hydroxide > pull with 800mL Xylene in 2 separate jars (400 each jar), whole mix is double boiled whole time. Xylene is so effective historically if hot in pulling damn near everything out with one pull if you use a fair deal for the pull. Tried second pulls many times, nothing came of it when using this much hot Xylene.

800mL total Xylene was defatted (mini-A/B) once, and only once, with 150mL vinegar mixed with 300mL water. That acidic water was then basified again, and pulled with just 500mL Xylene this time. Used FASA on this Xylene and it resulted in probably a total of 13g of fumarates.

Freebased by dissolving all the dried, (acetone washed) fumarates (13g) in minimal near-boiling water, then added sodium carbonate saturated water. About 4g of freebase goo floated to the top and the reaction was done in a few mins.

This end product is really, really oily I notice, and it's kindof a (light) tan color. Am I not doing nearly a thorough enough job defatting? Is it the case that even with perfect defatting, NMT can still make the end product refuse to crystallize no matter what? Thanks again for the help!

EDIT: Also, if it's sodium fumarate, any clue why that would be in my fumarates? Never heard of anyone with this issue