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DCM help & usage

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Z

Zorro

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There's so much talk on here about using DCM as the initial solvent but I've looked all over the forum and can't find much detail in its actual use compared to Naptha. It's mighty hard to get it over here although being a bit resourceful swims managed to get a couple of litres... HPLC grade it is... Would it need to be distilled first before use?

So, when doing a standard A/B tek with sodium carbonate, do you still do the same number of pulls, and what ratio of DCM to naptha would you use to collect the spice?

You don't use it to freeze precipitate and to extract the DMT you evaporate it down completely and use heptane which DMT is soluble in? Swims seen the tek to then separate the 5meo from the dmt. You say to use 10% citric acid / acetone solution so to make that is it 10g to 100ml acetone?

Once the DMT has been removed with MRHB, would you potentially be left with jungle spice? Swim also has xylene so would that be better for jungle? Reading the tek for that, you just continue to wash with heptane until no more DMT evaps out? I guess it will also pull DMT N-Oxide so how is this then separated, just point me to a link is theres one?

Would be great if you can just correct me if I'm wrong anywhere and help with the above questions... cheers... :d
 
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for starters, DCM sinks. for this reason, a sep funnel is a necessary tool.
HPLC grade is pure enough
and DMT isn't very soluble in heptane, thus why it's heated to dissolve the dmt, and freeze precipitated to collect it. dmt is actually much more soluble in dcm than heptane and naptha.

dcm can hold more dmt per unit volume, and doesn't need to be heated. multiple extractions aren't necessary, one good swirl is all it takes.

one could evaporate the dcm w/dmt in a dish, and recrystallize by pouring a minimal amount of hot heptane and let evap, or collect it and freeze precipitate

a couple notes: don't do a defatting step, if using dcm. you can do a regular a/b, or STB; if doing a/b, add basic sol'n directly to the acidic sol'n, until the pH gets up to ~ 9-10. then extract with dcm. if doing STB, take the pH to about 13, then extract with dcm.
remember, less dcm is required. if you have 500mL basic solution, about 75mL dcm should be enough.
 
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I was aware that it sinks but didn't realise the amounts were that small so I'll get a sep funnel for that to make it easier... Saves having to pour all the top off to get at it...

Don't know what it smells like but the reports say it's not good...
 
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dcm smells sweet, so does chloroform.

the amounts used aren't particularly small (SWIM wouldn't bother using any less than 25mL), but you're correct, working with a sep funnel makes the process a lot easier. swim prefers it over naptha because less amounts are used, and evap is quick. for this reason, it leaves a residue..just recrystallize with bestine
 
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