# Ephedrine extraction from plants



## G.Patton

*Introduction*​


Ephedrine was found in the Chinese "Ma-huang" or Ephedra sinica Stapf plant, made from various species of ephedra, by Nagai in 1887. It has two chiral centers so that four configurationally isomeric ephedrines exist. The two naturally occurring ephedrines differ in the configuration of the secondary alcohol group.

There are two methods of Ephedrine extraction. First one was taken from German patent and allow getting Ephedrine hydrochloride with high purity grade. This method is suitable for laboratory manufacturing more than for kitchen home lab. Second one is simple extraction method with ethanol and naphtha, which give quite dirty free base of ephedrine. Nevertheless, simple method may be carried out at home garage and product may be purified with recrystallization as in first method.​*Equipment and glassware:*

1000 mL x2; 250 ml x2 Beakers
100 mL x5; Erlenmeyer flasks;
Glass rod;
Glass column (d = 2.5 cm or wider, l = 70 cm);
Cotton ball;
500 mL round bottom flask;
Rotary evaporator;
500 ml Separating funnel;
Conventional funnel;
Filter paper;
Hydrogen chloride gas production apparatus;
Büchner funnel and flask;
Water-jet aspirator;
Laboratory scale (0.1 — 100 g is suitable);
Spatula.
*Reagents:*

Ephedra sinica Stapf 100 g;


Sodium carbonate (Na2CO3) 50 g;
Distilled water, 150 mL;
Dichloromethane (CH2Cl2) ~1500 mL;
Diethyl ether 50 mL;
Hydrochloric acid 150 mL (HCl 0.5 N);
Potassium carbonate (K2CO3) 50 g;
Sodium hydroxide aq. solution (NaOH 1 N) ~100 mL;
Sodium sulfate (Na2SO4) or magnesium sulfate (MgSO4) ~100 g;
Acetone 30 mL;
Methanol (MeOH) ~10 mL;
Activated charcoal (optional) ~1 g;




Soluble in H2O 47.62 g/L (25 ºC), alcohol, ether, chloroform, and oils;​Boiling Point: 255 °C at 760 mm Hg (free base);
Melting Point freebase: 37-39 ̊C;
Melting point HCI salt: 187-188 ̊C;
Molecular Weight: 165.236 g/mole;
Density: 1.124 g/cm3 (20 °C);
CAS Number: 299-42-3 (free base) and 50-98-6 (hydrochloride salt).

*L-ephedrine hydrochloride from ephedra herb [50-98-6] C10H15NO HCl*​*Determination of content **(optional):*
5 g of ground ephedra herb are mixed with 2 g of sodium carbonate and 7 mL of water and left to stand at room temperature for 3 hours. The mixture is treated three times with 50 ml of dichloromethane and stirred for at least 2 hours each time. The extract is pipetted off in each case. The organic phase is evaporated under vacuum (at 40 °C to 1 ml). After adding 20 mL of diethyl ether, it is extracted four times with 20 mL of 0.5 N hydrochloric acid, each time.

The combined hydrochloric acid phases are washed twice with 20 ml of ether, each time. After neutralization with 1 N sodium hydroxide solution (pH 7.5-8), it is extracted three times with 40 ml of dichloromethane and concentrated. The residue is taken up in 10 ml of water, and 3 ml of 0.1 N sodium hydroxide solution and 10 ml of 0.1 N I2/KI solution are added. The solution is stirred with gentle warming for 30 minutes. It is then carefully acidified with diluted HCl and a few drops of starch solution are added. The excess iodine is titrated with 0.1 N sodium thiosulphate solution until the color changes from blue to colorless.

*Extraction procedure:
1.* 100 g of powdered ephedra herb is added to a solution of 50 g of sodium carbonate in 150 ml of water in a 1000 ml beaker, mixed with a glass rod and left to stand for at least 2 hours.

*2.* A glass column (d = 2.5 cm or wider, l = 70 cm) is filled one third with dichloromethane and then filled in portions with the drug pulp. The drug should settle in the column without any air bubbles. The drug is covered with a glass cotton ball. (Please note: do not press the column filling too tightly).

*3.* It is percolated by continuously adding 1000 ml of dichloromethane (about two drops/sec). The percolate is concentrated portionwise in a 500 mL round bottom flask under vacuum to a volume of 5 mL.

*4.* 30 mL of ether are added to the extract, and it is shaken out three times with 50 ml of 0.5 N hydrochloric acid each time.

*5.* The combined hydrochloric acid extracts are filtered into a 500 ml separating funnel through a funnel with a pleated filter containing 50 g of potassium carbonate (add carefully). It must be filtered through carbonate slowly enough that the solution no longer reacts acidically (otherwise add carbonate). The carbonate is first rinsed with the methylene chloride for the extraction.

*6.* In this, the solution is shaken out four times with 75 ml of dichloromethane each time.

*7.* The combined organic phases are dried over sodium sulfate and concentrated in portions in a 250 ml flask on a rotary evaporator. The resulting yellow-orange oil is taken up in a mixture of 20 ml of diethyl ether and 20 ml of dichloromethane.

*8.* Dried hydrogen chloride gas is introduced into this solution. The apparatus for HCl generation consists of a multi-necked round-bottom flask with a stirrer, which is charged with sodium chloride and sulfuric acid (from a dropping funnel). To dry it, the gas is again passed through a washing bottle with a sodium chloride and sulfuric acid. The introduction into the alkaloid solution takes place with a Pasteur pipette. Empty safety washing bottles are installed in mirror image between all vessels so that no mixing can occur even if solutions are accidentally sucked back (see figure below). The excess gas is fed into a wash bottle with 10% NaOH solution (vent!).

*[G.Patton note:* You, probably, can substitute these *8-9* steps with addition of HCl conc. solution until precipitate stop forming. After, neutralize solution by NaOH aq solution to pH 7. Evaporate water under vacuum with minimum heating to get crystals.*]*​*

*​*9**.* After about 5 minutes, an off-white precipitate of alkaloid hydrochlorides forms. The supply of hydrogen chloride is stopped, and all hose connections are disconnected from to prevent the liquids from being sucked back.

*10.* The alkaloid mixture is filtered off using a Büchner funnel.

*11.* About 30 ml of acetone are added to a 250 ml beaker and the mixture is heated on a water bath while adding methanol (about 10 ml) in portions until residue has completely dissolved.

*12.* A spatula tip of activated charcoal is added, boiled and the hot solution filtered. Just enough acetone is added to the still hot filtrate until the crystals begin to precipitate.

*13.* The mother liquor is carefully pipetted off the product, which precipitates on cooling (at least 6 hours); the crystals are washed with a little acetone and air dried.

If there is still no TLC-uniform product, the product is dissolved in 15 times the amount of methanol, treated with 100 times the amount of acetone and recrystallized at about 4 °C overnight.​


> E. Stahl und W. Schild - Isolierung und Charakterisierung von Naturstoffen, Gustav Fischer Verlag 1986, S. 87-90 • J.A. Sanchez - Journal de Pharmacie et de Chimie, 22 (1935) 489



*Second (simplified) extraction way to Ephedrine free base*​*Equipment and glassware:*​
Pyrex pots ~750 mL x2;
Heating plate (or stove);
Filter with filter paper;
Sponge cake pan, 2.5 cm deep.
*Reagents:*​
Ephedra sinica Stapf;
Ethyl alcohol (EtOH) ~2.25 L;
750 mL Naphtha.
*1st step:*
*a)* Fine powder placed in a four quart Pyrex pot, about 750 mL of ethyl alcohol (EtOH) to cover the powder. For this process, use _Ever Clear_ from local spirit hut. The pot and alcohol to be warmed at ~32 °C (don’t bring to boil as it will destroy the Ephedrine). After allowing to steep for 10 minutes, remove the pot from the stove.

*b) *After 15 minutes filter the mush through a #15 gold filter with a coffee filter inside the gold filter (you can use a laboratory glass funnel or another filter sieve) then set the mush aside.

*c) *The filtered solution is poured into a 2.5 cm deep sponge cake pan covered with cheese cloth and allow to dry. Allow the solution to dry for 12 hours, leaving only a fine white powder (which shows to be 70% Ephedrine and 30% misc, mostly oils that the alcohol couldn’t break down).

*2nd step:
a) *Same as before, placed it in a four quart Pyrex pot. To the pot add 750 mL Naphtha, shake it vigorously 5-10 min and let it soak for three days.

*b) *Filter the mush the same way as above. Set the Naphtha solution aside for the second batch. Allow the mush to dry for three days.

*c) *Transfer the mush to a fresh Pyrex and cover with 750 mL ethyl alcohol, shake it vigorously 5-10 min and allow soaking for two days. Filter the mush, as you already know how to mark the solution “A” so that you can recognize it later.

*d) *Then place mush back in Pyrex and cover with another 750 mL ethanole this time, shake it vigorously 5-10 min and allow soaking for one day filter as you know how and then trash.

*e) *Now combine the second solution with the first into a 2.5 cm sponge cake pan to dry. Dry it for one day, leaving behind fine white powder.

Result 99% (not approved) Ephedrine free base, so total of Ephedrine extracted from *453 g* of Ma Huang is *96 grams*.​


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## PossumKid

Damn. Thank you for this write-up. Gives me a good reason to stop by the local TCM shop, and maybe let my soxhlet get a lil work done.


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## yuiopjkl

What can be used instead of Naphtha?


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## G.Patton

yuiopjkl said:


> What can be used instead of Naphtha?



yuiopjklYou can try another non-polar solvents such as hexane, cyclohexane, octane, heptane, pentane. They are suitable.


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## yuiopjkl

G.Patton said:


> leaving only a fine white powder (which shows to be 70% Ephedrine and 30% misc, mostly oils that the alcohol couldn’t break down).



G.PattonThanks for reply.

Is this the final powder?

And How can I make meth from it?


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## G.Patton

yuiopjkl said:


> And How can I make meth from it?



yuiopjkl


http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/index.php?threads/methamphetamine-from-ephedrine-tablets.302/


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## yuiopjkl

G.Patton said:


> You can try another non-polar solvents such as hexane, cyclohexane, octane, heptane, pentane. They are suitable.



G.PattonCan I use kerosene?


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## G.Patton

yuiopjkl said:


> Can I use kerosene?



yuiopjklYes, but make sure there are no other substances.


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## Needtolearn

any one have a link that sells this powder ?


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## yuiopjkl

G.Patton said:


> *1st step:*
> *a)* Fine powder placed in a four quart Pyrex pot, about 750 mL of ethyl alcohol (EtOH) to cover the powder. For this process, use _Ever Clear_ from local spirit hut. The pot and alcohol to be warmed at ~32 °C (don’t bring to boil as it will destroy the Ephedrine). After allowing to steep for 10 minutes, remove the pot from the stove.
> 
> *b) *After 15 minutes filter the mush through a #15 gold filter with a coffee filter inside the gold filter (you can use a laboratory glass funnel or another filter sieve) then set the mush aside.
> 
> *c) *The filtered solution is poured into a 2.5 cm deep sponge cake pan covered with cheese cloth and allow to dry. Allow the solution to dry for 12 hours, leaving only a fine white powder (which shows to be 70% Ephedrine and 30% misc, mostly oils that the alcohol couldn’t break down).​



G.PattonI did this method.

When the alcohol begins to evaporate I see white powder.

But when I let it dry, I found a lot of oils.
Yield: 10% ephedrine, 90% oil.

Any advice ?


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## G.Patton

yuiopjkl said:


> Yield: 10% ephedrine, 90% oil.
> 
> Any advice ?



yuiopjklYou have to cool it in a fridge, after, take a fork or something like this and rub the bottom of the Pyrex dish with oil. Rubbing allows making crystals immediately because make crystallization centers. Make it with the cooled solution.​


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## yuiopjkl

G.Patton said:


> You have to cool it in a fridge, after, take a fork or something like this and rub the bottom of the Pyrex dish with oil. Rubbing allows making crystals immediately because make crystallization centers. Make it with the cooled solution.​



G.PattonDo you mean that I make the solution evaporate to half and then put it in the fridge so that the layer of oils collects on top and then I dispose of it?


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## G.Patton

yuiopjkl said:


> Do you mean that I make the solution evaporate to half and then put it in the fridge so that the layer of oils collects on top and then I dispose of it?



yuiopjklno, i made advice for making crystals in current situation, instruction in topic is correct


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## yuiopjkl

G.Patton said:


> You have to cool it in a fridge, after, take a fork or something like this and rub the bottom of the Pyrex dish with oil. Rubbing allows making crystals immediately because make crystallization centers. Make it with the cooled solution.​



G.Pattoncan you explain more :
Cooling the solution( which is 90% oils) to what temperature?

When stirring, will the oil separate from the ephedrine?

Is it stirring when all the ethanol has evaporated?


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## G.Patton

yuiopjkl said:


> Cooling the solution( which is 90% oils) to what temperature?



yuiopjkl~2-5 deg. C.


yuiopjkl said:


> When stirring, will the oil separate from the ephedrine?


yes, i think it would be better to do


yuiopjkl said:


> Is it stirring when all the ethanol has evaporated?


correct, with rubbing


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## Alper192535

Thanks


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## Microogata

Thank you very much for this information. I was wondering where I could get my hands on this Ephedra (or Ma-Huang) plant ? 
Do you think that Alibaba is a good source to buy it from (since it comes from China) ? https://www.alibaba.com/trade/search?fsb=y&IndexArea=product_en&CatId=&SearchText=ma-huang


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## G.Patton

Microogata said:


> Thank you very much for this information. I was wondering where I could get my hands on this Ephedra (or Ma-Huang) plant ?
> Do you think that Alibaba is a good source to buy it from (since it comes from China) ? https://www.alibaba.com/trade/search?fsb=y&IndexArea=product_en&CatId=&SearchText=ma-huang



MicroogataI'm not sure. It depends on laws in your country and custom service there.


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## raw

When I finish with no powder but oil. Can I go directly from this oil to meth by Hi/P reaction? And can I use toluene as solvent for extracting ephedrine from plants?


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## G.Patton

raw said:


> When I finish with no powder but oil. Can I go directly from this oil to meth by Hi/P reaction?



rawHave you tried to crystallize oil by freezing and rubbing (rub bottom by glass rod)? You can, if you are sure that it is ephedrine.


raw said:


> And can I use toluene as solvent for extracting ephedrine from plants?


You can try. But I'm not sure.


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## raw

Frozen and friction (rubbing bottom with a glass rod)? Thank you . I didnt try this. After this process, the crystallization should form stable even at room temperature after being pulled out of the fridge?


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## G.Patton

raw said:


> After this process, the crystallization should form stable even at room temperature after being pulled out of the fridge?



rawYes, look at Melting point on the top of this post.


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## lililibetfan

interesting information


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## raw

About ephedra plants... Where can I found it ? Does anyone have experience that grows in a country in Europe? For example, in the south? In Croatia ?


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## PewPew411

I've tried this multiple ways mentioned here and other places and only gotten a sludge that tests negative with a Chen-Kao reaction.


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## G.Patton

PewPew411 said:


> I've tried this multiple ways mentioned here and other places and only gotten a sludge that tests negative with a Chen-Kao reaction.



PewPew411Have you done them with an absolutely similar conditions? Are you sure that your raw plants are contain ephedrine? Probably you've got just weed grass.


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## PewPew411

Quality of ephedra is unknown I've got some 10:1 and regular plant material from china 
I followed this exactly but at 50% volume with the extract and when gassing out it just turned dark with no precipitate 



https://www.thevespiary.org/rhodium/Rhodium/Vespiary/talk/files/4762-writeupd9b9.PDF?topic=2723.0



Alcohol extractions and other experiments with the plant matter have lead no where. I'm going to try the writeup on the straight plant matter next and see how I go 
I might run a ghetto soxhlet extractor using a pressure equalizing addition funnel with condenser to pump chloroform through the plant matter


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