Your analysis of this reagent combination and extraction path

[Light-Being]

Hi friends,

I'd appreciate it if a few of you seasoned vets could look over the following somewhat atypical reagent combination for extraction and tell me if you see any glaring problems:

[with powdered MHRB]
- BLAB-style non-heated acid soak in phosphoric acid solution
- Basify to 9.5 with sodium carbonate
- Extract with DCM
- Salt combined DCM extractions with FASW
- Separate the FASW/product layer and evaporate its water to collect the spicy fumarate salt

Mainly I'm wondering if there are any incompatibilities anywhere between the reagents. This specific combination of path and reagents isn't one that I've seen mentioned, yet it seems like it's one that would work very well---unless I'm missing something big.

If the scheme looks okay, I'd appreciate knowing that. I'd also love any recommendations for volumes of things (at a scale of 454g MHRB.)

Thanks so much,
LB

 

[endlessness]

Raise the PH more than 9.5, if you use sodium carb maybe get it closer to 11.

The rest seems like it could work but I never worked with DCM. Definitely recrystalize/wash your fumarates with IPA/Acetone to remove DCM traces, you dnt want to be ingesting that.

I would say at least a gallon container for that quantity. Maybe better a bit less mimosa (like lets say 350g) for a gallon container just to prevent any problems of it being too thick. So adding mimosa+water+acid till nearly the top, leaving space for the non-polar pull.

 

[Light-Being]

Hi endlessness,

Thanks for replying. You know what, the reason I mentioned only going to 9.5 was that I had just read somewhere that with DCM as the extraction solvent, you actually only do have to go to 9.5 instead of pushing it to 11 as is done with naphtha. It said that the alks are 5X more soluble in room temp DCM than they are in even hot naphtha, and at lower pH.

But then, later I read that sodium carbonate is a pain because it takes way too much of it to get alkaline enough (and thus too much water volume to dissolve it). So I'm sort of off that kick now. I really don't mind using NaOH... it always works.

What I'm wondering now is, if NaOH is used, does the same thing still hold true about DCM (its ability to extract the alkaloids at only 9.5) or does one go all the way to 11 anyway?

I guess the attractive combo now is phosphoric acid + NaOH + DCM

Thanks for the tip on washing the fumarates to rid them of DCM. I would have thought that since DCM is so very volatile, it could not get trapped in crystals, but wouldn't want to bank on that.

Now I just have to double check for any incompatibilities between DCM and fumaric/fumarates. One thing about DCM for sure is that plastic vessels are a no-no. Glass only.