PoorMansChemist profile
PoorMansChemist
PoorMansChemist
Chemistry experiments and demonstrations with a focus on making unusual and not often seen compounds.
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PoorMansChemist
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Hey guys sorry I've been out of commission for so long. My laptop got wrecked about a month ago and that made making new videos difficult. I got my old laptop working and all of the new software is installed on it so I'm hoping this will do for the time being. I still need to get the fans replaced. All of the dust out here in the lab has killed them over the years. 
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PoorMansChemist
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A little something for my loyal subscribe star supporters. You guys are fucking amazing. Now you kids behave yourselves. This is merely posted for your academic edification. The prep comes from a paper on optimizing the synthesis and characterization of DMT by reductive amination using a GC-ITMS analysis. The paper is called Characterization of the Synthesis of DMT by Reductive Amination Using Gas Chromatography Ion Trap Mass Spectrometry. The second part comes from the United Nations Bulletin on Narcotics on a webpage called Analytical Separations of Mixtures of Hallucinogenic Drugs. It's available online. 

I compiled all of this information myself. The DMT prep is the highest yield one from the paper and should give yields around 75-78%. Purification afterwards is probably required since it produced some weird nitrile compounds that probably don't occur in nature and if they do I can't find any literature on them or what they do to humans. Be careful here. They could cause brain damage for all I know. Not to mention that doing this prep is probably wildly illegal to do pretty much everywhere but Antarctica or the Moon. Again I post this merely for your intellectual edification. Be good. ;-)

Synthesis of N,N-Dimethyltryptamine By Reductive Amination
  1. 1 gram of tryptamine was dissolved in forty milliliters of ice cold methanol that is chilled in ice water
  2. Next 1.26 grams of glacial acetic acid and 629 milligrams of sodium cyanoborohydride are added to the tryptamine solution. 
  3. While continuing the ice water cooling stir the mixture for 5 minutes.
  4. 858 milligrams of an aqueous 39% (w/v) solution of formaldehyde dissolved in 10 mL of methanol is added dropwise to the reaction mixture over a period of 20 minutes. 
  5. The ice was removed and the reaction was left to stir for two and a half hours at room temperature.
  6. 3 mL of a 20% NaOH solution is added to the reaction mixture with stirring.
  7. The solvent is removed under reduced pressure. 
  8. 20 mL of distilled water is added to the residue in the flask and the mixture is extracted three times with 20 mL portions of chloroform (do not use dichloromethane as DMT reacts with DCM).
  9. Combine the chloroform extracts and wash it once with 20 mL of water and then with 20 mL of brine.
  10. Dry the chloroform solution with anhydrous magnesium sulfate. 
  11. Filter off the MgSO4 and wash the cake twice with 20 milliliters of fresh dried chloroform.
  12. Evaporate off the chloroform under reduced pressure.
  13. The oily residue is dissolved in absolute ethanol and sprayed onto a suitable plant base such as cannabis or tobacco. Allow the plant matter to completely dry in a cool, dark place. The product is then ready for use.
  14. This method was taken from "Characterization of the synthesis of N,N-dimethyltryptamine by reductive amination using gas chromatography ion trap mass spectrometry" 

TLC Analysis of The Common Tryptamine Hallucinogens
  1. Silica gel plates are activated by heating for 2 hours at 100 degrees Celsius and then stored in a desiccator until required for use. 
  2. The solvent system to be used was prepared the day before. After mixing and shaking the solvents in a separatory funnel they are allowed to equilibrate and separate into layers overnight. The next day drain off the organic phase and discard the aqueous layer if one is present.
  3. The developing chambers are lined with filter paper the mobile phase is added and they are then sealed using a paste made of starch and glycerol. If the mobile phase contained ammonium hydroxide a 50 ml beaker was partially filled with ammonium hydroxide and placed in the chamber after the mobile phase had been added. The chambers are then allowed to equilibrate for 3 hours.
  4. The drug sample is spotted 3 cm from the bottom of the plate and at least 2 cm from its edges. Individual samples are run at least 2 cm apart. The sample should be spotted as evenly as possible. To dry the sample before developing a gentle stream of nitrogen or argon can be used.
  5. The previously spotted plates are placed in the equilibrated chamber for developing and removed when the solvent front reaches the 15 cm mark. All separations are conducted in a constant temperature room.
  6. The plates are then allowed to air dry after which they are viewed under ultra-violet light and the results recorded. Following this observation the plates are heated for 5 minutes at 110 degrees Celsius to remove any trace of alkaline vapors. 
  7. For qualitative data the plates are sprayed copiously with a solution of p-dimethylaminobenzaldehyde (125 mg in 100 ml of 1:1 sulfuric acid and 2 drops of a 10% ferric chloride solution). With the p-dimethylaminobenzaldehyde spray the characteristic colors of the individual drugs appear following an additional 20 minutes of heating at 100 degrees C.
  8.  For quantitative data the plates are sprayed copiously with a solution of potassium iodoplatinate (3 ml of a 10% platinum chloride solution mixed with 97 ml water to which is then added 100 ml of a 6% solution of potassium iodide). The advantage of the iodoplatinate spray is that although the resulting colors are only variations of brown a spot may be scraped from the plate and reduced with sodium sulfite after which the drug may be appropriately redissolved. 
  9. For the mobile phase benzene-ethyl acetate-diethylamine (7:2:1) and using p-dimethylaminobenzaldehyde as an indicator as described above psilocybin has an Rf value of 0.00 and produces a navy blue spot. Mescaline has an Rf value of 0.16 and produces a light brown spot. LSD has an Rf value of 0.29 and produces a clear blue spot. Dimethyltryptamine has an Rf value of 0.42 and produces a deep blue-green spot. Ibogaine has an Rf value of 0.55 and produces a dirty yellow-green spot.
  10. For the mobile phase n-propanol-5% ammonia (5:2) psilocybin has an Rf of 0.08, mescaline has an Rf of 0.55, LSD has an Rf of 0.71, DMT has an Rf of 0.70, and Ibogaine has an Rf of 0.72.
  11. For the mobile phase methanol-ammonium hydroxide (100:1.5)psilocybin has an Rf of 0.04, mescaline has an Rf of 0.23, DMT has an Rf of 0.34, and LSD has an Rf of 0.60.
  12. For identifying DMT ethanol-25% ammonia (1:3) gives an Rf value of about 0.60 and for acetone-chloroform (4:1) it's 0.11.
  13. For identifying mescaline Ethanol-pyridine-dioxane-water (50:20:25:5) gives an Rf of 0.18. Ethyl alcohol-acetic acid-water (60:30:10) gives 0.81. Both ethanol-dioxane-benzene-25% ammonia (5:40:50:5) and methanol-n-butanol-benzene-water (60:15:10:15) give an Rf of 0.30.
  14. For identifying psilocybin n-propanol-5% ammonia (5:2) and n-butanol-acetic acid-water (2:1:1) both give Rf values of 0.15.
  15. For identifying LSD dichloromethane-methanol (93:7)gives an Rf of 0.60 for LSD base. Acetone-chloroform (4:1) gives an Rf of about 1,1,1-trichloroethane-methanol (90:10) 0.40 gives an Rf of 0.55 for LSD base.
  16. This method was taken from "Analytical separations of mixtures of hallucinogenic drugs"
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PoorMansChemist
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Holy sheep shit, ladies and gentlemen, I think I just figured out a way to deal with the copious amounts of HCN gas needed to make pure TlCN solution. TlCN can be precipitated from a solution of thallous nitrate by addition of aqueous potassium cyanide but the yield sucks. TlCN is NOT all that insoluble despite the way the literature reads. 100 grams of water dissolves 8.67 grams at 0°C, 15.17 grams at 14°C, and 29.57 grams at 31°C. The other way to make TlCN is to bubble HCN through a solution of TlOH. This reaction has to be done way back away from the house but up until now I've had serious concerns about going near it to adjust anything and especially breaking down the apparatus. HCN is lighter than air but not by a whole lot so I would imagine that it rises slowly. That gives me pause. But apparently this whole problem can be solved quite easily by simply breathing through a very long garden hose whose far end is way way away on the other side of the property. So long as I breathe in through my mouth and out through my nose I think it will work. I should stress this is only to buy me enough time to make whatever adjustment needs to be made or to open the apparatus to degas at the end. Sure in principle this should work perfectly. In practice having tried something similar already in the past I know its not quite that easy. But I think I can pull it off. Obviously don't try this at home kids. 
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PoorMansChemist
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Seriously Atomistry?
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PoorMansChemist
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Damn it. I am out of both aqueous ammonia and nitric acid. I can make up a batch on one tonight and a batch of the other tomorrow. But it's supposed to piss rain for the next two days. I was going to do diamminedichloropalladium(II). I still might. I would just need to bubble some of the NH3 from the ammonia generator through the suspension of PdCl2. It makes a dark tan precipitate in water. Atomistry describes it as a "flesh colored precipitate". While it is indeed what anyone today would call a flesh tone I'm not sure if someone in Europe a century ago (which is when and where I think the source material comes from) would call it "flesh colored". I'm not saying it's "muh systemic racism" or anything like that. I'm just saying that people looked at things differently a century ago and I'm trying to put myself in their heads. Anyways we could go a different way with this and make up palladous sulfide PdS, filter it, dry it, and then fuse it with 12 parts KOH and 12 parts S powder to make potassium thiopalladite K2Pd3S4. I have more than enough fuel for an H2S generator. Either way I have to set up a gas generator.  
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PoorMansChemist
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The next organic video will be out within the next week. I'd also like to do a short video on the oxythallation reaction since it's such a neat trick. The next prep video will be the diammoniate of palladium(II) chloride PdCl2(NH3)2. After that I want to do a prep of palladous sulfide and from that make potassium thiopalladite K2Pd3S4 which is supposed to be a violet-blue turning gray when it dries. That sounds pretty neat. Not sure what we will do with the diammoniate. Maybe use it to make bis(acetonitrile) palladium(II) chloride if possible. It would finally give me something useful to do with all this ACN. 

This is how I will make the diammoniate. This comes from the Atomistry page for palladium dichloride. "When palladium dichloride is dissolved in water, and ammonia added in sufficient excess to dissolve the flesh-coloured precipitate, the diammoniate, PdCl2.2NH3, may be obtained as a precipitate by diluting with a large volume of water and acidulating with hydrochloric acid. It may be dried at 110° to 120° C., and has been used for the determination of the atomic weight of palladium. Density 2.5."
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