blue.magic
Rising Star
MOTIVATION
I really hate evaporating solvents as well as lengthy pipetting that never removes all the solvent. On the other hand, I like working with lab glassware. This tek is more suitable for amateur (basement) chemists than kitchen alchemists because of more equipment is needed, but I hope it will be of some interest. Also I just like to share how I do it.
I started using separatory funnel and a distillation apparatus for A/B extraction of DMT. This works great as one is able to remove the solvent layer very precisely, combine the pulls and cleanly distill off the solvent (thus recycling it). The reduced solvent is then poured into a Pyrex dish and left to cool as with traditional freeze-precipitation schemes.
Now one more improvement came to my mind. Why not use DCM as a solvent? First, it forms a bottom layer and thus the pulls can be quickly taken from the separatory funnel while keeping the mother liquor inside the whole time. Second, it has a low boiling point allowing for easy distillation with just a hot water bath.
DCM does not allow freeze precipitation (AFAIK) but we can use small amount of naphtha for this while removing all the DCM.
THE TEK
NOTE: When water is mentioned, it is filtered or distilled.
Grind 250 g MHRB in a cofee grinder, add to a pressure cooker, cover with 1 600 ml of water.
(optional) You can also break down the bark further by covering it with 600 ml water in a Tupperware dish, mix intimately with a fork, then freeze and thaw it 1-3 times. Finally, add everyting to a pressure cooker with additional 1 000 ml water to top it up to the final 1 600 ml.
Pressure cook for 20-30 minutes.
Filter the liquid through a coarse and then fine sieve to separate the solids (bark). Keep extraction liquid in one large enough pot (more will be added) and return the bark to a pressure cooker.
Cover the back with 1 500 ml water, boil (now without a lid) for 20-30 minutes.
Repeat filtering and boiling once more, combine all the water extractions in one pot.
(optional) Transfer the bark to a cheesecloth and squeeze out any remaining liquid.
(optional) The bark in a cheesecloth can be soaked in warm/hot water and squeezed again to remove any trapped actives.
Let the soup sit overnight.
Decant as much clear supernatant liquid as possible to a separate pot, transfer the rest in a cheesecloth and squeeze out any remaining liquid.
(optional) The bark in a cheesecloth can be soaked in warm/hot water and squeezed again to remove any trapped actives.
Reduce the liquid by boiling it down to approx 1 200 - 1 500 ml.
While still hot, add approx. 100-120 g of sodium chloride (non-iodized table salt).
Let the soup cool down a bit.
(optional) De-fatting: Transfer the liquid to a 2 000 ml separatory funnel and extract four times with 50 ml DCM. Discard the DCM.
Transfer the soup to a 2 000 ml beaker.
Add approx. 100 ml of 50% sodium hydroxide solution while stirring.
Heat up the soup to 45 °C.
Transfer the now warm/hot soup to a 2 000 ml separatory funnel.
Extract four times with 50 ml DCM. Combine the DCM pulls. Discard the soup (prefferably neutralize the soup first with acid, boil off any remaining DCM, then let it cool down and only then pour it down the drain).
(optional) You can wash the DCM with slightly basic water or brine in a 250 ml separatory funnel. I use 1% ammonia solution with some salt in it.
To a 500 ml round bottom flask equipped with a stirrer, add the combined DCM pulls, add 40 ml naphtha.
Set up a simple distillation apparatus with hot water bath and an ice bath.
While stirring, heat up the water to 60-80 °C (temperature should be high enough so the DCM will boil off, not too vigorously, but low enough so it's safely below the boiling point of naphtha).
When no further boiling is observed, stop the distillation, remove the boiling flask and pour the naphtha into a Pyrex dish.
Seal the dish and let it stand few hours at room temperature, then few hours in the fridge and finally 12+ hours in the freezer.
Pour off the naphtha, dry the crystals with fan while keeping the dish upside down for 20-30 minutes.
Scrape the crystals.
(optional) Wash the crystals with small amount of 1% ammonia solution.
Crush the crystals (if possible) and further air-dry or vacuum-dry them to remove any trapped naphtha or DCM.
NOTES
I have not determined the best amount of naphtha but that depends on how rich the bark is. Ideally, one can start with small amount (say 20-30 ml) and if the solution is cloudy or shows precipitation, even at 80° C, add small amounts of naphtha until everything is dissolved. The goal is to make a supersaturated solution. This will readily crystallize upon cooling.
The DCM and naphta will end up cross-contaminated to a small extent and may need to be further purified if intended to be used separately.
I am not sure about the solvent washing with basic brine (e.g. 1% ammonia). When doing mescaline extraction, this washing seems to help picking up some discoloration.
EXPERIMENTAL
To be added later.
I really hate evaporating solvents as well as lengthy pipetting that never removes all the solvent. On the other hand, I like working with lab glassware. This tek is more suitable for amateur (basement) chemists than kitchen alchemists because of more equipment is needed, but I hope it will be of some interest. Also I just like to share how I do it.
I started using separatory funnel and a distillation apparatus for A/B extraction of DMT. This works great as one is able to remove the solvent layer very precisely, combine the pulls and cleanly distill off the solvent (thus recycling it). The reduced solvent is then poured into a Pyrex dish and left to cool as with traditional freeze-precipitation schemes.
Now one more improvement came to my mind. Why not use DCM as a solvent? First, it forms a bottom layer and thus the pulls can be quickly taken from the separatory funnel while keeping the mother liquor inside the whole time. Second, it has a low boiling point allowing for easy distillation with just a hot water bath.
DCM does not allow freeze precipitation (AFAIK) but we can use small amount of naphtha for this while removing all the DCM.
THE TEK
NOTE: When water is mentioned, it is filtered or distilled.
Grind 250 g MHRB in a cofee grinder, add to a pressure cooker, cover with 1 600 ml of water.
(optional) You can also break down the bark further by covering it with 600 ml water in a Tupperware dish, mix intimately with a fork, then freeze and thaw it 1-3 times. Finally, add everyting to a pressure cooker with additional 1 000 ml water to top it up to the final 1 600 ml.
Pressure cook for 20-30 minutes.
Filter the liquid through a coarse and then fine sieve to separate the solids (bark). Keep extraction liquid in one large enough pot (more will be added) and return the bark to a pressure cooker.
Cover the back with 1 500 ml water, boil (now without a lid) for 20-30 minutes.
Repeat filtering and boiling once more, combine all the water extractions in one pot.
(optional) Transfer the bark to a cheesecloth and squeeze out any remaining liquid.
(optional) The bark in a cheesecloth can be soaked in warm/hot water and squeezed again to remove any trapped actives.
Let the soup sit overnight.
Decant as much clear supernatant liquid as possible to a separate pot, transfer the rest in a cheesecloth and squeeze out any remaining liquid.
(optional) The bark in a cheesecloth can be soaked in warm/hot water and squeezed again to remove any trapped actives.
Reduce the liquid by boiling it down to approx 1 200 - 1 500 ml.
While still hot, add approx. 100-120 g of sodium chloride (non-iodized table salt).
Let the soup cool down a bit.
(optional) De-fatting: Transfer the liquid to a 2 000 ml separatory funnel and extract four times with 50 ml DCM. Discard the DCM.
Transfer the soup to a 2 000 ml beaker.
Add approx. 100 ml of 50% sodium hydroxide solution while stirring.
Heat up the soup to 45 °C.
Transfer the now warm/hot soup to a 2 000 ml separatory funnel.
Extract four times with 50 ml DCM. Combine the DCM pulls. Discard the soup (prefferably neutralize the soup first with acid, boil off any remaining DCM, then let it cool down and only then pour it down the drain).
(optional) You can wash the DCM with slightly basic water or brine in a 250 ml separatory funnel. I use 1% ammonia solution with some salt in it.
To a 500 ml round bottom flask equipped with a stirrer, add the combined DCM pulls, add 40 ml naphtha.
Set up a simple distillation apparatus with hot water bath and an ice bath.
While stirring, heat up the water to 60-80 °C (temperature should be high enough so the DCM will boil off, not too vigorously, but low enough so it's safely below the boiling point of naphtha).
When no further boiling is observed, stop the distillation, remove the boiling flask and pour the naphtha into a Pyrex dish.
Seal the dish and let it stand few hours at room temperature, then few hours in the fridge and finally 12+ hours in the freezer.
Pour off the naphtha, dry the crystals with fan while keeping the dish upside down for 20-30 minutes.
Scrape the crystals.
(optional) Wash the crystals with small amount of 1% ammonia solution.
Crush the crystals (if possible) and further air-dry or vacuum-dry them to remove any trapped naphtha or DCM.
NOTES
I have not determined the best amount of naphtha but that depends on how rich the bark is. Ideally, one can start with small amount (say 20-30 ml) and if the solution is cloudy or shows precipitation, even at 80° C, add small amounts of naphtha until everything is dissolved. The goal is to make a supersaturated solution. This will readily crystallize upon cooling.
The DCM and naphta will end up cross-contaminated to a small extent and may need to be further purified if intended to be used separately.
I am not sure about the solvent washing with basic brine (e.g. 1% ammonia). When doing mescaline extraction, this washing seems to help picking up some discoloration.
EXPERIMENTAL
To be added later.
