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G.Patton

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Introduction

Purification at home condition is one of the hottest topics in the drug market. Example: you have a substance with a smell and color which is quite far from ideal. Unfortunately, it happens unacceptably often. Heavenly stuff do not come from every hellish cuisine, and we will pay special attention to the permanent giant of stimulants - amphetamine.

Amphetamine on the market is most common in various forms: sulfate and phosphate, rarely - hydrochloride. Sulfate - a salt of sulfuric acid (H2SO4) - more often. Phosphate - a salt of phosphoric acid (H3PO4) - less often. These two forms have a stable state of aggregation, do not require special storage conditions (unlike the hydrochloride salt) do not lose their properties for years, have the same presentation and, most importantly, are quite easily absorbed by the body. There is different topic about Amphetamine salts. The qualitative effect of amphetamine differs slightly between these salts. The ingredients in the synthesis of amphetamine must be balanced, only then the quality of the effects and product characteristics will be the same wherever the drug is produced.

In any synthesis, only toxic and dangerous substances are used. There are no other options. The color of amphetamine is white (a barely noticeable cream or gray tint may be present), the smell is completely absent, the taste is bitter. Fine-grained powder, dry, homogeneous, not oily, solubility in water without residue. Omitting more detailed characteristics, let's consider the most simple cleaning method "Product Washing" and the advanced method "Acid-base Extraction".


Method one: Acid-base extraction

Acid-base extraction (ABE), as a purification method, allows you to get a high-quality drug. Methods for using available reagents, tools and instruments.

Definitions:
  • Rm - reaction mass
  • NaOH - caustic soda
  • MgSO4 - magnesium sulfate
  • DCM - dichloromethane
  • amph - amphetamine
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1. Dissolve amphetamine salt in water 1:1 (by weight). Complete dissolution should be achieved. It may be necessary to warm the solution, add water. Insoluble precipitate, crumbs, particles are removed by filtration.
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2. Add 50% NaOH solution to pH 12 with small portions. A solution of NaOH in distilled water (room temperature) is poured by drops, depends on the volume. When pH 12 is reached, an oily layer (amphetamine free base) forms on the top surface of Rm. The amount of amphetamine base is equal to the mass of dissolved amphetamine. The color can be from amber to transparent, depending on the purity of the salt.
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3. Pour petroleum ether (20% by volume) into Rm and mix thoroughly. Let the layers separate. The ether is insoluble in water, as is the free base, but the base is soluble in ether. In this way, we remove some of the water-soluble impurities from amphetamine.
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4. Separate the top layer with the extract into an another container using a plastic / glass syringe or separating funnel. If DCM was used instead of petroleum ether, then we separate the bottom layer. Avoid the ingress of water into the separated extract.

5. Wash the water (the remaining lower layer) with petroleum ether three times (5% of the water volume).

6. Combine the extracts.
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7. Dry the extract with anhydrous MgSO4 for 1 hour, placing it in the freezer. The glass should be hermetically sealed.

MgSO4 is added to Rm 3-20% (depends on amount of water there) of the volume of ether. Drying is necessary to remove the remaining water from the ether, which in further stages, by dissolving the amph salt in water, will lead to a lower (by weight) yield of pure product. You can wrap it with cling film for container tightness. It must be closed to avoid saturation of the solution with moisture concentrating in the freezer. If MgSO4 is not available, keep Rm in the freezer for 12 hours. Then, in case of formation of water at the bottom of the container (in a layer or drops), the ether should be carefully decanted (poured out) without touching the water.
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8. We filter the extract from MgSO4 that has absorbed water using a vacuum pump connected to a Buchner funnel with a Bunsen flask and a paper filter. You can use a conventional filter without vacuum, which will slightly reduce the yield (you have to wash the filter with an anhydrous solvent). The solution should be decanted onto the filter without lifting the sediment from the bottom. MgSO4 remaining at the bottom of the beaker has to be washed with an anhydrous solvent (pour it onto a filter) and disposed of.
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9. We evaporate the ether extract by 2/3 by heating it to 40 degrees using an electric stove (WITHOUT FLAME!). It is difficult to determine the pH level in ether solution with further addition of acid, so we reduce volume to a possible minimum. It doesn't be worth to heat the solution above 40 degrees, since a (albeit small) part of the free base of amphetamine can be evaporated with the ether. Evaporation should be carried out away from fire and in a well-ventilated area. Inhaling ether vapors is extremely harmful to health. In the presence of a rotary evaporator, evaporation should be carried out in it.

Important note: In no case should you evaporate the ether using a fan, directing it into the container with the extract. The extract is dry (without water) and actively absorbs moisture from the air. The fan directs the flow of air, which somehow has a percentage of moisture. A couple of minutes will saturate the ether with water, forming an aqueous phase at the bottom of the container.
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10. We dilute Rm with dry cold (from the freezer) acetone (in half the volume). Acetone is needed to bind the remaining water and facilitate mixing.
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11. We acidify Rm to 5.5 pH using H2SO4 solution in acetone (1:1) with thorough mixing. Additionally, we add acetone in small portions as the solution thickens.
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Amphetamine salt is formed. Sulfate if H2SO4 is used or phosphate if H3PO4 is used.
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12. Filter the resulting salt. Before that, tightly closing the glass, you can place it in the freezer for several hours. Low temperatures promote acceleration of crystallization.

13. Without removing the filter, rinse the salt three times with small portions of acetone.
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Optionally, you can additionally recrystallize the amphetamine salt from alcohol or vodka according to classical methods.

Discussion

The number of impurities in amphetamine can reach a very high percentage. An indicator can be not only the presence of any smell, shades of color, salt moisture, but also poor solubility in water. Read Amphetamine assessment protocol. Contaminants may be deposited, in an insoluble layer or solid particles, depends on their nature of origin. The final yield of pure amphetamine obtained by ABE can reach both 80% and 5% of the original weight.

For one of the examples of a possible case, let's take a sample (Sample No. 2) from the next part of the article.
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Initially, the amphetamine salt had a light orange color, with a characteristic pungent odor and a moist, oily consistency, and was washed with dry acetone (or IPA). Having become almost white and having lost a significant number of impurities in weight, the salt almost lost its smell and became a loose consistency.
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We achieved a good result with help of Product Washing procedure (second part). But it is not. The subsequent biotest (zero tolerance) subjectively showed extremely low (at the placebo level) activity of the substance at nasal dosages of 130 mg and 80 mg (four subjects in different weight categories). Side effects are expressed slightly. Further, the ABE of this amphetamine salt was carried out.
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The mixture began to thicken, forming fine whiskers after complete dissolution in water (Rm = 6 pH) after approximately five minutes. Further separation of the phase with the extract was difficult because the solution turned into a porridge.
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The addition of water volumes to Rm did not have a significant effect on solubility - the mass tended to occupy the entire space. Filtering an aqueous solution through a paper filter is difficult (the paper disintegrates), and the Schott filter has not been tested. Nevertheless, it was possible to complete the extraction, but with an extremely low percentage of pure amphetamine in the yield. Its biotests showed high activity in dosages of 60 mg.


Method Two: Product Washing

Drug washing is an essential and final part of almost any synthesis. Sometimes repeated several times. The method is available to anyone, does not require skills, can significantly improve the quality of product and presentation. The method is Ideal for small quantities. Washing is indicated for residues of F2NP, alkalis, acids and so on. Washing will not remove contaminants (acetaminophen, caffeine, etc.) and mercury salts.

The most accessible, and therefore easier, is to wash amphetamine with isopropyl alcohol (IPA). More difficult to use is anhydrous acetone. IPA does not contain water, and therefore it does not dissolve amph salt. The key to the process success is the lack of water. It is needing for avoiding amph from dissolution with pollutants because they will be thrown out.

We take our amphetamine and put it into a beaker. Thoroughly grind into a dust and add IPA ~5-10 volumes of powder. After mixing, let it stand for 5-10 minutes. The alcohol (or acetone), impurities and amphetamine in the beaker now. It is necessary to apply a filtering method to separate them. From improvised means for squeezing the mass, a white dense fabric is suitable. You can also simply draw a fraction with pollutants with a syringe. If the amount to be purified is less than half a gram, then it is more convenient to carry out the entire procedure in a Petri dish. After allowing to settle, carefully drain the solvent (alcohol or acetone), leaving the amphetamine. Removing the solvent with impurities should leave the amphetamine to drying to a constant weight (and no smell). In the pictures we can see the whole simple process.

We will consider two samples
  • Sample number 1, although it seems white, but only in comparison with the second sample. Light beige color. Distinct odor of amphetamine free base.
  • Sample number 2 has an oily texture, a pronounced orange color and a strong smell of vinegar. The smell of vinegar and color indicate the absence of even primary cleaning. With a probability of 100%, this sample contains impurities (salts of mercury, aluminum, P2NP, etc.).
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For the curiosity sake, after placing the samples in the IPA and letting it settle, we will measure the pH.
  • Sample No. 1 - pH not less than 8. This indicates that the crystallization step (adding acid to a solution of amphetamine free base in acetone) was not completed. A strong burning sensation while consuming is guaranteed.
  • Sample No. 2 - pH is ideal, equal to 6.
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Start the cleaning procedure

1. Sample No. 1 is placed in a syringe with IPA and mixed thoroughly. After settling, you can see a crystalline sediment at the bottom. Probably dealer added impurities. Drain the liquid fraction.
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2. Compare the sample with the original by drying the washed sample to constant weight. It became lighter and lost its smell. Approximately 4% weight loss.
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1. Sample No. 2 is placed in a beaker with IPA. Mix it thoroughly. Letting it settle, drain the IPS. You can also squeeze out amphetamine with a cloth. The image shows that the sample has a denser fraction at the bottom and a less dense fraction above.
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2. The procedure was repeated 8 times with this sample, only then the amphetamine became significantly lighter.
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Approximately 25% weight loss.
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We compare the result after drying these fractions separately to constant weight. We didn't receive the white sample. As you can see, the fractions have a gray tint - these are organic impurities that do not dissolve and are not removed by washing. This amphetamine is still unusable. To thoroughly clean it up, it is necessary to carry out an acid-base extraction (ABE).
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Summarizing, we can once again be convinced of the importance of such a stage as washing the final product with anhydrous acetone or IPA. The use of amphetamines of various colors can cause serious harm to the body and psyche.

Conclusion

The amphetamine originally sold was not only of the lowest quality, but could also cause significant harm to the health of a user. In particular, it affected those who use the drug intravenously (i.v.). After dissolution of the powder in water for injection (if this could be achieved at all), the solution thickened in the syringe, making it difficult to inject into the bloodstream. Ignorance of consumers is used (intentionally or not) by sellers in the sale of defective drugs batches, harming the body and psyche of the consumers, and bringing profit to sellers. In conclusion, it is important to note that the lack of experience with pure drugs leaves the buyer incompetent in assessing the quality of the product purchased.

 
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cyb3r0

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Is there a video explanation?
 

Pussy_Kurt

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Nice Workout :) Has you ever think about rectification of your amin oil? After rectification you get about 98 - 99 % chemical purity, look at the fraction. When i can trust my budy who made for me an analysis with HPLC an Mass-Spektro.

LUdqTamjCR
 

diogenes

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Hi Patton, in section 10, the text says to add acetone in half the volume, however, looking at the next picture the volume is much larger, about 4 times as much as before? How much Acetone are we supposed to add?
 

ASheSChem

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stupid question..
is there a difference in the effect of consumption between sulfate and phosphate amphetamine?
 

diogenes

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Sulphate contains more amphetamine by weight than phosphate, because the phosphate molecule is larger (bigger proportion of the amphetamine salt). So if you take equal amounts say 100mg of each then the Sulphate should be stronger. Some people also say that Sulphate absorbs/kicks in faster on the other hand Phosphate gives less fluctuations, the plasma levels are more steady. I personally prefer Sulphate I think, but best is probably to test your preference (it is quite easy as you can just simply use a different acid at the last step of synthesis).
 

ACAB

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stupid question..
is there a difference in the effect of consumption between sulfate and phosphate amphetamine?
Should not be so, the psychoactive substance is the amphetamine, the salt has no effect.
 

DocX

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Nice Workout :) Has you ever think about rectification of your amin oil? After rectification you get about 98 - 99 % chemical purity, look at the fraction. When i can trust my budy who made for me an analysis with HPLC an Mass-Spektro.

View attachment 3719
This is interesting! I am not familiar with the term or the process, could anyone with knowledge take a little time to explain it?
 

ASheSChem

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i have phosphate acid 81% (19% water) ; it would be ok to trying the acidification of freebase ?
 

ACAB

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i have phosphate acid 81% (19% water) ; it would be ok to trying the acidification of freebase ?
I'd say there's too much water in it, or is amphetamine phosphate not water soluble? The loss will be too great.
 

Mclssmxxl

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Coincidence has it I tried h3po4 yesyerday.I had 50ml H3PO4 in which 2 additional gram of it’s anhydryde were dissolved.I drove reaction to the end, extracted ipoh with xylene, dried over anhydrous mgso4 for 10-15 minutes.The somewhat dry xylene with freebase was transfered to a clean dry glass.1,15 of the Phosphoric acid were added dropwise to 20-40ml of acetone.And nothing precipitated, sadly.I dont know if my acid was bad or the anhydride messed things up but I ended up wasting 3g of Raw mats. C’est la vie
 

G.Patton

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I dont know if my acid was bad
Have you tried to scrub by glass rod the bottom surface of glass with this mixture to make centers of crystallization? Have you cooled this mixture?
 

Mclssmxxl

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Have you tried to scrub by glass rod the bottom surface of glass with this mixture to make centers of crystallization? Have you cooled this mixture?
No, mixture was used at room temp with only a little agitation of the container beforehand.I will do this next time and report back.I will also source some fresh conc. orthophosphoric acid to compare.Thanks mr patton.
 

ASheSChem

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11. We acidify Rm to 5.5 pH using H2SO4 solution in acetone (1:1) with thorough mixing. Additionally, we add acetone in small portions as the solution thickens.
it is really 1:1 ? 1ml acetone for 1ml acid sulfuric?
i ask beaucause in the amph synthesis it is 10:1
 

ACAB

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i ask beaucause in the amph synthesis it is 10:1
The ratio is freely selectable whether 1:1 1:4 or 1:10, the thinner the sulfuric acid the more solution is needed to neutralize. Some also use 2 different solutions, at the beginning 1:1 and when nearing pH6 take a thinner solution, because it is easier to adjust the pH6 without overacidification. Keep in mind that the thicker the H2SO4 solution, the greater the risk of temporary acidification, you must add the solution very slowly to avoid this.
 
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