Ratios of RB to DMC, Lye and deionized water

[littlemouse]

Hey guys

So I have a few questions, anyone, here willing to help

I decided to pick methylene chloride as an acid-base because of it's Xlogp compared to xylene and toluene (lighter fluid or naphtha) but what ratios of deionized water, lye, Mimosa RB and methylene chloride do you guys suggest?

I was thinking of using 50g root, 500ml water, 10g lye, Should I use the same amount of methylene chloride as I would the naphtha (which was 50ml) I don't know if I should use more or less of anything, would help greatly getting it spot on so i don't waste anything

I have safety glasses, breathing mask, coveralls and safety gloves, a magnetic stirrer hot plate, a conical flask with stopper, 1 liter, glass pipets, and coffee filters
My method would be deionized water with lye and root bark, leave stirring with magnetic stirrer for an hour, Add in methylene chloride turn upside down a few times, leave it until it polarized and methylene chloride is then pipetted into either a pyrex dish, or used jam jar, frozen to help crystals overnight, filter through coffee filter/filter paper, leaving it to dry, Then after drying I'll do a recrystallization with heptane (both crystals and heptane in a separate glass containers which sit within a 50 degree water bath) when it reaches hand-hot levels, pipet heptane into crystal and swirl around until dissolved, Then take it out, sit to cool for a moment, freeze and finally filter again, then leave to dry.

I pretty much spent two days, going through some of the extraction guides but wanted a final say from you lovely people, I've already learnt so much here and I can tell i'm going to learn a WHOLE lot more

This is my first time doing this, So any extra advice, tips, and help would be appreciated, I don't wanna end up killing myself haha!

 

[padawan]

Do you have a PH meter, or at least test strips? The PH levels are what you're aiming for - the relative ratios of base to acid soup in the teks are all a bit rough and as per the tek authors experience. My experiences have been different (ie. X grams of whatever mixed into Y ml of whatever doesn't come out at the same PH as the teks tend to suggest). PH test and add your base slowly until you reach the desired PH.

 

[leratiomyces]

There a few problems with your method.

Your bark will slowly accumulate at the bottom of the vessel after you stop stirring. That's where your methylene chloride ends up after you stop stirring or shaking. At the bottom. When you pipette out your dcm, there will be bark particles in it.

Secondly, even if there were no bark particles, it's a pain in the bum to pipette out the bottom layer of a biphasic solution.

Thirdly, dmt will not precipitate out of dcm at low temperature.

And as padawan suggested, make your your solution is very much basic before you extract.

 

[littlemouse]

There a few problems with your method.

Your bark will slowly accumulate at the bottom of the vessel after you stop stirring. That's where your methylene chloride ends up after you stop stirring or shaking. At the bottom. When you pipette out your dcm, there will be bark particles in it.

Secondly, even if there were no bark particles, it's a pain in the bum to pipette out the bottom layer of a biphasic solution.

Thirdly, dmt will not precipitate out of dcm at low temperature.

And as padawan suggested, make your your solution is very much basic before you extract.

Wait why will the methylene chloride sink? Shouldn't it float to the top like other solvents?

I don't mind if there are a few bark particles in it, That's what the Heptane recrystallization process is for as far as I'm aware, to remove impurities.

Do you have a PH meter, or at least test strips? The PH levels are what you're aiming for - the relative ratios of base to acid soup in the teks are all a bit rough and as per the tek authors experience. My experiences have been different (ie. X grams of whatever mixed into Y ml of whatever doesn't come out at the same PH as the teks tend to suggest). PH test and add your base slowly until you reach the desired PH.

No, but I can easily get some, I'm using 99% caustic soda, As far as I'm aware it's not an acid at all, It's an alkaline, What PH should the Lye and Deionized water solution be when I add in my root bark?

 

[downwardsfromzero]

Wait why will the methylene chloride sink? Shouldn't it float to the top like other solvents?

Density.

I don't mind if there are a few bark particles in it, That's what the Heptane recrystallization process is for as far as I'm aware, to remove impurities.

Recrystallisation is not intended as a work-around for pure sloppiness.

How are you planning to get the alkaloid back out of your DCM? (Assuming you manage to recover the DCM.)

Have you ever used DCM for anything before?


I'm a bit concerned about your apparent level of aptitude, TBH.

 

[littlemouse]

Wait why will the methylene chloride sink? Shouldn't it float to the top like other solvents?

Density.

I don't mind if there are a few bark particles in it, That's what the Heptane recrystallization process is for as far as I'm aware, to remove impurities.

Recrystallisation is not intended as a work-around for pure sloppiness.

How are you planning to get the alkaloid back out of your DCM? (Assuming you manage to recover the DCM.)

Have you ever used DCM for anything before?


I'm a bit concerned about your apparent level of aptitude, TBH.

I assume that you cannot read too well, I told you this is my first time, So yes, you be concerned about my apparent level of aptitude, or you can help improve it by giving help, which is what I asked for and what you haven't done.

Also, I would be able to remove it with a Pepit, In the same way as if the methylene chloride floated or not, And the alkaloid can be filtered from the solvent through a process of freezing, filtering and drying. As I stated above UNLESS, of course, you're telling me I CAN'T do that, IN which case you could state WHY and HOW I can achieve this, Which is what the point of this post was LITERALLY about.

 

[leratiomyces]

Hi littlemouse

In the spirit of assisting you, if this is your first extraction, you are better off following one of the methods on the wiki.
Less will go wrong.

If you are set on the method you suggested, then the following is relevant,
Dmt will not precipitate out of cold dcm, toluene, or xylene. In all three cases you will need to evaporate all the solvent off, and then recrystallise your product with an appropriate solvent (hexane, heptane, naphtha).
As downsward said, the density of dcm is greater than water, so it sinks.
A sep funnel would allow you to remove the bottom layer of a biphasic solution much more easily than a pipette.
Dcm reacts with dmt when they are left in contact with each other for extended periods of time.
Dcm is such a great solvent that it extracts more compounds than you want, and can therefore make the steps that follow, more difficult.

Hope that helps

 

[littlemouse]

I'ld also like to point out, that all the information in my introduction post was gathered HERE, on this site, So maybe it's a reflection of a few days reading what substances would be best to achieve the results I wanted, and there are a number of people here who recommended Methylene Chloride over Ligther fluid, Would you like to take it up with them and explain to them how wrong they are, Or just me who collected my information from people such as yourself?

 

[padawan]

No, but I can easily get some, I'm using 99% caustic soda, As far as I'm aware it's not an acid at all, It's an alkaline, What PH should the Lye and Deionized water solution be when I add in my root bark?

Aim for about PH 12-13 after you do your STB with NaOH. Slowly add the NaOH saturated H20 to the bark, and if you have a PH meter then watch it settle to a stable level. If you have PH paper then check it after stirring for a few minutes. Going too high with the PH really isn't much of an issue with DMT though, but personally I like to leave a bit of room and raise the PH after each subsequent pull (and after several cumulative days or even weeks have elapsed since the initial basify)

 

[littlemouse]

Hi littlemouse

In the spirit of assisting you, if this is your first extraction, you are better off following one of the methods on the wiki.
Less will go wrong.

If you are set on the method you suggested, then the following is relevant,
Dmt will not precipitate out of cold dcm, toluene, or xylene. In all three cases you will need to evaporate all the solvent off, and then recrystallise your product with an appropriate solvent (hexane, heptane, naphtha).
As downsward said, the density of dcm is greater than water, so it sinks.
A sep funnel would allow you to remove the bottom layer of a biphasic solution much more easily than a pipette.
Dcm reacts with dmt when they are left in contact with each other for extended periods of time.
Dcm is such a great solvent that it extracts more compounds than you want, and can therefore make the steps that follow, more difficult.

Hope that helps

This is the type of help I was looking for, Thank you very very much, Ok so when i'm using the DCM inside my lye solution mixed with powdered root bark, I would have to do this on a heat, It is why I have a heated magnetic stirrer, What heat would you recommend to not burn any of the substances.

I'll look into Sep funnels instead of the Pipettes, I can see that it would be useful for removing bottom layers instead of top layers, So might need to invest in one, Thanks very much for that.

DCM shouldn't remain in contact with DMT for too long then? Would it be better to only leave it as long as it separates the DMT and then filters it right away instead of freezing since freezing will not help the process of precipitate?

I was using DCM for its quickness compared to the multiple extractions naphtha, But since it will also extract compounds I do not want, would that be where the heptane comes into play which I thought was to purify through recrystallization.

 

[littlemouse]

Ok so from what I've gathered from the replies, I've edited my plan a little.

- 50g root bark (Frozen and then ground)
- 500ml deionized water
- 10g lye (use a litmus test for pH 12)
- 50ml Methylene chloride
- 50ml Heptane (will only need enough to cover crystals)

- Safety Glasses, a breathing mask, and coveralls
- Magnetic stirrer hot plate with stir bars
- 1-liter conical flask with stopper
- 1-liter Separation funnel
- 500ml Glass beaker
- Some jam jars
- Glass pipettes
- Coffee filters
- Litmus test

My method would be,
- use 500ml beaker for 500ml deionized water add in slowly 10g lye (or litmus test till pH 12)
- add root bark 50g to the Conical flask, add the lye solution
- Place on the magnetic stirrer with a stir bar for an hour
- Add in 50ml methylene chloride, leave it until it polarized and methylene chloride sinks

(How would I get it into the Separation funnel, would pouring it in and then just waiting for it to polarize again be ok?)

- Use the Separation funnel tap and filter methylene chloride layer through coffee filters into a jam jar, Leave the coffee filters to dry.

Then after drying, I'll do a recrystallization with heptane

- Put both crystals and 50ml heptane in a separate jam jars
- Place within a 50-degree water bath
- pipette heptane when hot enough into crystal and swirl around until dissolved.
- Remove both jars. sit to cool for a moment, freeze and finally filter again, then leave to dry.


feel free to add anything else I might need to do to help my process, Thanks very much!

 

[downwardsfromzero]

I assume that you cannot read too well, I told you this is my first time, So yes, you be concerned about my apparent level of aptitude, or you can help improve it by giving help, which is what I asked for and what you haven't done.

Did I personally insult you?

I'm genuinely concerned about your abilities in handling dangerous chemicals, with which you intend to produce a CONTROLLED DRUG. I'm more interested in ascertaining that your level of experience in handling hazardous solvents and corrosive chemicals is sufficient that you don't get yourself into a dangerous situation.

I'ld also like to point out, that all the information in my introduction post was gathered HERE, on this site, So maybe it's a reflection of a few days reading what substances would be best to achieve the results I wanted, and there are a number of people here who recommended Methylene Chloride over Ligther fluid, Would you like to take it up with them and explain to them how wrong they are, Or just me who collected my information from people such as yourself?

Judging by your apparent lack of understanding of chemistry, I'd suggest you hold off on the extraction until you thoroughly understand the principles behind it. Do I really need to sugar coat this? That I give a damn about some random on the internet getting hurt?

Forgive my harsh tone, this is what comes of having spent my childhood years teaching myself chemistry - at the expense of having any social skills.
My view is that if a kid can teach him/herself chemistry, so can you.

And I didn't even have the internet back then :?:



Anyhow, here are some hints you'll have found a bit harder to have tracked down:

so when i'm using the DCM inside my lye solution mixed with powdered root bark, I would have to do this on a heat

What heat would you recommend to not burn any of the substances.

First check the boiling point of DCM.

Then make sure you don't mix it with powdered root bark. This is OK when doing STB with naphtha; with DCM you are going to end up with a toxic, emulsified mess. At least if you really insist on using DCM, do an A/B extraction. And if boiling up an acidic tea, be aware that MHRB is full of tannins that will precipitate on cooling. Patience is key in this step.

DCM forms emulsions relatively easily, especially with alkaline solutions. If your base soup is too concentrated, its density gets too close to that of DCM, making it very difficult for the NP solvent to separate out of the extraction mixture. Particulates only make this situation worse.

Leave your acidic tea to stand in the fridge for a day or two until it is crystal clear (it will be coloured, I mean no suspended solids here).

Dmt will not precipitate out of cold dcm, toluene, or xylene. In all three cases you will need to evaporate all the solvent off

It's also possible to extract the DMT out of these solvents using an acid. One needs to be wary that some salts of some organic compounds are soluble in DCM. I don't know if this includes DMT acetate but it could do. Mindlusion might know.

Once DMT has been recovered from an organic solvent into an aqueous acidic solution, if you want to Smoalk it it needs to be converted back into a freebase. A popular method of doing this is by using sodium carbonate and acetone.

IMO, it's best if you can avoid having to evaporate (or use) DCM, especially if it's your first attempt at extracting DMT.

 

[littlemouse]

Not sure how you got I was insulted, I said yes be concerned for me, But help raise me instead of acting better, You can always teach a person more you know, I'm adequate at chemistry, I may not be some type of unsocial expert since my studies went move into the path of physics and mathematics but I do alright, Also you said you taught yourself as a kid, I'm actually still a kid, and if you didn't have internet back then, I assume you a very old and have the experience to share.

This is just the first time doing a DMT extraction and I want to get everything exactly right down to the last detail, I have worked with dangerous chemicals many times in the past, But not like this, Normally to clean and stuff (caustic soda/lye).

So you suggest I do an acid-base extraction with pH 2 first before lye, Would vinegar work here or would I need something a bit stronger? Is there a method you can direct me to which you would think is most suitable for my current method so I can amend it? I read up that some DMT binds to the tannin, You say patience is key so I'm guessing I want to let it cool so I can get tannin, would that be correct?

I was using this as a basic guide, But I'm guessing changing the solvent would have to change the whole method.


Also, I though the acetone was only to make it into a fumarate to orally ingest it with an MAOI, You sure I need to turn the DMT-heptane into a fumarate?

 

[littlemouse]

DMT Extraction Overview - DMT-Nexus Wiki

wiki.dmt-nexus.me

here tells me i can do a STB with NaOH and then DCM, as long as I only gently swirl it instead of shake it....


"• Straight to Base Extraction – This method seems to have become the popular way to extract from Mimosa hostilis root bark, probably in part due to the low total extraction time reported in the Lazy Man’s Tek and other straight-to base methods. The basic idea is to simply cover the root bark with water basified to pH ~13 and pulverize the material, creating an aqueous solution in which the DMT freebase is not very soluble. An excess of hydroxide is used in order to physically break down the bark and allow the DMT to be exposed to nonpolar solvent. Sodium hydroxide is by far the most popular choice, though potassium hydroxide could be used instead. When going this route, a basic polar wash on your nonpolar solvent is practically a must; otherwise, some residual lye seems to remain in the product, making it more harsh. In the US, NaOH is a watched chemical due to its use in meth production. Ordering online or buying with a credit card could have undesired concsequences.


2. Nonpolar Extraction of the Freebase
At this point it’s time to recover your DMT freebase into a nonpolar solvent. Xylene and toluene are not recommended for this step, particularly with Mimosa, as they will carry along a red pigment that can end up in your final product (some people extract with these solvents with the explicit intent of extracting the red pigment, which has been reported to be psychoactive itself). Naphtha is the most commonly used solvent for this step, but diethyl ether, methylene chloride (DCM) and hexanes have both been used successfully as well. Remember when extracting, you want to swirl or gently mix the layers, not shake them. Nasty emulsions can form, which are to be avoided at all costs."

• Straight to Base Extractors – Your solution is already basic, so you’re good to go on this step. Just extract your basic, bark-filled mixture with several volumes of nonpolar solvent and pool the extracts.




^ So i can go STB with lye and then use DCM as the NP solvent... I don't need to A/B for it?

 

[downwardsfromzero]

That looks like a misuse of context. DCM can be used as a non-polar solvent at the base stage, but it would not be wise to use it in STB for the reasons already detailed. That entry in the wiki can't be take as definitive:

but diethyl ether, methylene chloride (DCM) and hexanes have both been used successfully as well.

The incongruous use of the word "both" here strongly suggests that one of those solvents was pasted into the sentence without sufficient forethought... And, on grounds of chemistry, there's more than a 1 in 3 chance that it was DCM added as the afterthought here. So if you really want to risk an unsuccessful first extraction in order to test out the veracity of that information, feel free. It would at least be a contribution to our field of knowledge.

If, on the other hand, you want to extract some DMT there are three choices: stick with STB and use your heptane as the NPS; do an A/B and use the heptane; or do an A/B and use the DCM. If you do choose to stick with using the DCM, it's worth investing in a separatory funnel first. (And if you have a separatory funnel it's worth having a ring stand for it.)

Also, I though the acetone was only to make it into a fumarate to orally ingest it with an MAOI, You sure I need to turn the DMT-heptane into a fumarate?

Acetone isn't just for fumarates. If you were to backsalt your DMT from the DCM into vinegar, it would be wise to allow it to evaporate to be sure of removing traces of DCM. It's then possible to convert back to freebase using sodium carbonate paste. After drying, the freebase can be recovered with acetone.

You'll probably be fine with a mini A/B using heptane, so long as there's no DCM present in sufficient quantity to mess up the freeze precip.


[Clear thinking after my bedtime comes at a substantial premium.]

 

[littlemouse]

Could you provide me with links to backsalting DMT from DCM into vinegar, Also what would be the best way to evaporate traces of DCM, just leaving it out to evaporate by itself? and then mixing with Sodium Carbonate paste leaving to dry and acetone?

Also yeah I have myself a ring stand and SF, I read somewhere that if I make the Aquaeous lye solution denser through salting, the DCM would float to the top, but that doesn't matter so much with an SF, and do I NEED to do anything to the DCM DMT extraction other than letting it evaporate if I don't want, and what would be the results?

Thanks for sharing your knowledge with me, learning quite a bit here

 

[leratiomyces]

I think downwards has summarised things quite well for you in their post above.

DMT Extraction Overview - DMT-Nexus Wiki

wiki.dmt-nexus.me

here tells me i can do a STB with NaOH and then DCM, as long as I only gently swirl it instead of shake it....


"• Straight to Base Extraction – This method seems to have become the popular way to extract from Mimosa hostilis root bark, probably in part due to the low total extraction time reported in the Lazy Man’s Tek and other straight-to base methods. The basic idea is to simply cover the root bark with water basified to pH ~13 and pulverize the material, creating an aqueous solution in which the DMT freebase is not very soluble. An excess of hydroxide is used in order to physically break down the bark and allow the DMT to be exposed to nonpolar solvent. Sodium hydroxide is by far the most popular choice, though potassium hydroxide could be used instead. When going this route, a basic polar wash on your nonpolar solvent is practically a must; otherwise, some residual lye seems to remain in the product, making it more harsh. In the US, NaOH is a watched chemical due to its use in meth production. Ordering online or buying with a credit card could have undesired concsequences.


2. Nonpolar Extraction of the Freebase
At this point it’s time to recover your DMT freebase into a nonpolar solvent. Xylene and toluene are not recommended for this step, particularly with Mimosa, as they will carry along a red pigment that can end up in your final product (some people extract with these solvents with the explicit intent of extracting the red pigment, which has been reported to be psychoactive itself). Naphtha is the most commonly used solvent for this step, but diethyl ether, methylene chloride (DCM) and hexanes have both been used successfully as well. Remember when extracting, you want to swirl or gently mix the layers, not shake them. Nasty emulsions can form, which are to be avoided at all costs."

• Straight to Base Extractors – Your solution is already basic, so you’re good to go on this step. Just extract your basic, bark-filled mixture with several volumes of nonpolar solvent and pool the extracts.




^ So i can go STB with lye and then use DCM as the NP solvent... I don't need to A/B for it?

This section you have found, is not the most well written information.
There is the suggestion that naphtha, diethyl ether, dcm and hexanes have all been used in a stb. I doubt anyone has done a successful stb with dcm. If they have, I hope they read this post and describe their method and results, for your sake.
Secondly there is the suggestion that toluene and xylene would extract a greater number of compounds and pigments, compared to dcm. This is highly improbable. A dcm extract from a stb is much more likely to contain a greater number of compounds and will be very dark in colour. Probably the same colour as the aqueous phase. I have tried to wash the filtered, acid extracts of bark with dcm, and this was certainly the case. A very dark organic phase that was difficult to separate.

Finally, this website is clearly a combination of many people's experiments and techniques, who come from many different countries and have access to many different chemicals, or limited access, I should say. Therefore you are not always going to get the same advice from every person. No different to any other discussion forum.

 

[littlemouse]

Hey down, Can you send me a tek for A/B and then DCm thanks

 

[littlemouse]

I think I might do the STB heptane for my first extraction, but I'm still on this DCM extraction because of what I've read up, but I'll have to get some acetone and sodium carbonate for the DCM, which I'll likely take your advice and do it through acid-base instead, I'll have to refine the tek though, Thanks very much for teaching me

 

[downwardsfromzero]

Mäuschen, just do the STB w/ heptane. You'll be much happier.

When you've got used to how extractions run in general, then you can start tinkering within the lesser-trod ground.

I can't link to any "teks" but I do know that I found them by looking for them. But maybe there was less information washing around back then. Category:Extraction Tek - DMT-Nexus Wiki

Many solvents can be used to extract DMT from plant materials, dichloromethane (Methylene Chloride, DCM) is good one but difficult to acquire at high purity without other solvents mixed into it without special ordering from a chemical supply house. If you do use DCM this solvent is heavier than water and instead of floating on top of the aqueous mix will go to the bottom and may cause a problem due to the basified water being pushed out of the root bark and difficult to separate from this solvent later. [emphasis added] [referring to use in STB]

Don't worry too much about the sodium carbonate/acetone bit - allowing the DMT vinegar to evaporate, then dissolving it in DIW followed by basing and pulling into heptane for freeze precip would also get rid of DCM residue.