Xylene FASA questions (jungle spice-fumarate)

[n0thing]

1. I understand you are supposed to dissolve fumaric acid in acetone and then add that acetone to the dmt saturated xylene but why is that if you dump fumaric acid in xylene and then add pure acetone to the xylene that the acetone wont absorb any more of the fumaric acid? Because of this, I am wasting a lot of acetone as i have to keep adding more (despite already heating the acetone to absorb more fumaric acid).

2. Why does junglespice-fumarate precipitate out of the xyxlene as a really fine powder/goo? I am worried about whether jungle spice is stealing saturation in xyxlene because i am not seeing dmt-fumarate crystals anymore that i did from my naphtha pull days where it would go naphtha pull -> evap -> acetone conversion to dmt-fumarate which leaves very crystal like dmt-fumarate crystals.

 

[endlessness]

1. It probably wont work and you'll have a bunch of undissolved fumaric acid at the bottom, mixed with maybe some dmt fumarate. And since fumaric acid is not very soluble in acetone, and the acetone will mix with xylene, I dont think you'll be able to get rid, of the fumaric acid excess by just adding acetone to that mix.

Also, you should not add warm FASA to the mix, but rather room temp FASA. Warm acetone might hold more fumaric acid which could precipitate together with your DMT.

2- Likely because you are probably adding the FASA too fast instead of dropwise over a few hours. Also if your FASA is warm, that may also be a reason

 

[n0thing]

1. It probably wont work and you'll have a bunch of undissolved fumaric acid at the bottom, mixed with maybe some dmt fumarate. And since fumaric acid is not very soluble in acetone, and the acetone will mix with xylene, I dont think you'll be able to get rid, of the fumaric acid excess by just adding acetone to that mix.

Also, you should not add warm FASA to the mix, but rather room temp FASA. Warm acetone might hold more fumaric acid which could precipitate together with your DMT.

2- Likely because you are probably adding the FASA too fast instead of dropwise over a few hours. Also if your FASA is warm, that may also be a reason

Thanks for the reply endlessness. Just to clarify, why is it that acetone won't absorb fumaric acid when it is dissolved in xylene? Chemically i don't see how to this is works?

Also, once the major jelly has precipitated out of the xylene, i get some more clouding when i keep adding FASA but this doesn't crystallize. It just settle to the bottom as a very very very fine powder that isn't filterable. I am wondering if i should just evap the xylene as I am unsure whether I am getting all the DMT out with FASA

Also, why add dropwise? Should i just add till the jelly stops precipitating, filter that and then add dropwise for the finer unknown cloudy stuff?

 

[endlessness]

Regarding why acetone wont absorb excess fumaric acid, because you are not talking about acetone anymore, you are talking about a mixture of acetone+xylene, which behaves differently than pure acetone would.

Regarding your jelly/goo, another possibility is that your acetone is wet. It is important to make sure the acetone is totally dry, because if wet, things will be messed up. Is the acetone from a good chemical supply provider? Can you read the labels, does it say how pure it is?

Considering the acetone is dry, the reason to add dropwise is similar to why you can grow bigger crystals when evaporating slowly instead of fast: The slower is done, it gives time for a small amount of small crystals to form first, and then as more crystals start precipitating, they tend to gather on top of the smaller crystals forming bigger crystals, and so on. If you add it all quickly (same as if you evap solvent quickly), then you are forcing DMT to crystalize before it has time to grow on top of other crystal, so it forces it to be small crystals/powder.

What you should probably do at this point to make sure you recover all your alkaloids now is to separate your bottom goo from your xylene. Then you should make sure you have all your fumarates from the xylene by washing it with water a couple of times and evapping that on a water bath. Whatever you have left will be excess fumaric acid+some DMT+some impurities. Then you can put this together with the goo you separated earlier, and proceed to recrystalize/purify it in any number of ways (for example you can mix it with sodium carbonate and a bit of water to make a paste, let it dry, then pull with acetone/ipa and do FASA/FASI again but this time adding the FASA/FASI very slowly and making sure you have dry acetone/IPA).

Hope that helps