So I had an experiment a while back of directly methylating MDA. The formaldehyde to imine and al/hg reduction worked but with horrible yields. 2 grams distilled freebase gave ~600 mg acetone washed salt. The point is, I was trying to find a way to tlc and seperate the primary from secondary amine. Doping my eluent with triethylamine and running on silica didn't work. I made some crappy alumina plates and iodine staining did seem to show something but it didn't really work either. I can't find my notes to see what solvent system I used.

Fast forward and I'm on a totally different experiment but again find myself wanting to tlc the same secondary amine. Not to separate mda but I'm looking for a way to chromatograph mdma freebase for purification in general. I have since obtained some good UV reactive alumina plates and I have a container of alumina for running a column.

Does anyone have suggestions on a solvent system for mdma freebase on alumina stationary?

As thevespiary is unreachable I'm not being able to find the procedure anywhere else, has anyone of you saved a copy of it?

I ordered some p2np and couldn't immediately use it so I stored it in a refrigerator. The product came in an alluminium bag but I placed it in an airtight container in case the bag was damaged.

How long can I keep it at this condition and temperature before it degrades considerably?

I already stored it for two months (excluding 15 days of shipping). I'm not sure if I can still use it for synthesis. The purity(HPLC) was claimed to be >=99% by the chemist.

Sorry for the newbie question. I couldn't find any reliable info about it on the internet.

Edit: freezing is not feasible right now

I know, be patient and it'll be up again, just asking if anyone has any info. I swear I'm backing it up this time, I can't handle the stress and anticipation

please do consider that i do not test these products save for the law would romp me ;'(

Condensing black pepper and ylang ylang oil yielded 6hr action salvinorins

It looks like well think how salvinorin is to crystal dilaudid and acid.

this would look crystalled like morphine and mushroms but there was no nitrogen during formation.

I used sodium metasilicate if you get something less tasty but crazy from borax or even a nicer syrup from some other silicate let me know.

The procedure seems simple enough in theory, but some of these chemicals just sound sketch and wish there was another way around it. Mainly, from melatonin to 5-MeO-T seems simple, but why is sodium Bisulfate needed? I understand the deacetylation (I think) but wouldnt this be relatively similar to decarboxylation? Sodium bisulfate is pretty easy to make, so im not worried about that. The main parts that come into play is the methanol (toxic), formaldehyde (toxic) and NaBH4 (probably also toxic and explosive).

My main question is if there are any other synthetic pathways from 5-MeO-T. Would methyl iodine work or is it just as dangerous if not more than NaBH4? all the materials other than the formaldehyde and NaBH4 seem relatively hard to get, and would probably raise an eyebrow or two online?

If anyone has simple procedures for making the chemicals needed or substitutes, let me know!

(same thing for LSA --> LSD, would ethyl iodine work?)

I'm not going to post a recipe, but I do want to share a couple of steps to some fascinating possibilities:

.

Citronellal -> Helional Transformation

Starting material: Citronellal, from the citronella plant

Oxidation process: Citronellal is oxidized (typically using oxidizing agents such as ozone or peracetic acid).

Product: Helional (via 3,7-dimethyl-6-octenal), a compound with an extended alkene chain and a distinctive odor profile.

.

Biocatalysis – Aldoxime to Amide

Prepare Reaction Solution- dissolve Helional aldoxime in ethanol-buffer (1:1 ratio).

Add the nitrile hydratase enzyme solution. (Rhodococcus rhodochrous)

Incubation: Keep at 30°C with gentle shaking for 6-12 hours.

Monitor pH (keep near neutral, 6.5-7.5).

Check for Amide Formation- use TLC (thin-layer chromatography) or HPLC to confirm amide production..

.

Amide to Amine Conversion via Amidase

Add Amidase Enzyme (From Same Bacteria or Another Source)

Some Pseudomonas species secrete amidases that efficiently hydrolyze amides to amines.

Alternatively, use a separate hydrolysis step with a mild base (pH 9-10, NaHCO₃ buffer).

Incubate at 30°C for Another 12-24 Hours.

The reaction progresses at a moderate rate without heat.

I'm no chemist, but I'm an enthusiastic. I'm wondering how people attach the various acyl groups to the nitrogen of lysergamides.

Sorry for the basic question, but I asked a while back on the vespiary, and I feel like more information could have been provided.

My best information was that they used various anhydride and ketenes to attach the groups, but idk, as I'm not a chemist.

Can someone please elucidate this for me? I greatly appreciate any help, and apologize for the basic nature of this question.

~~~====~~~~~~==========\/\\\\\////\/==========~~~~~~====~~~

~~~====~~~~~~5-(EtO/AcO)-DET + 4-(EtO/AcO)-DET~~~~~~====~~~

~~~====~~~~~~==========*^#^*^#*^#*^#==========~~~~~~====~~~

~~~====~~~~~~==========)()()()()()()==========~~~~~~====~~~

~~~====~~~~~~========##(pure,yieldy)##========~~~~~~====~~~

~~~====~~~~~~==========&&&&&&&&&&&&&==========~~~~~~====~~~

1.cyclize indole:

-from benzyl alcohol isopropyl and ammonium chloride 1:1:1, as after the previous mixture (makes a sterically activated polyol):

-add 2mol NaHCO3 to cyclize 1-ethylindole then add ammonium chloride with MgSO4 again and 2M ethanol/methanol already there and yield DET or DMT freebase pure with 1M MgCl2

very weird ion exchange chemistry as it avoids all alcohol substitutions and creates a NH-sterically protected indolylethane

author talk: if it was NH2 it wouldnt be able to form the second amine if you study acid aliphatics

the reason this works:

you just add sodium acetate and drop in HCl or Ammonium Chloride to get respectively 4 or 5 acetyl DET/DMT

afaict you yield about 1/3 of the other (4 or 5) position in both of those cases if you have 1M water present

so remember you should do these in solvents of a stronger alcohol (methanol or even just formaldehyde if using methanol to get methyl)

ITS ALL BECAUSE OF SIDE-CHAINED STERIC INHIBITION AND REDOX CYCLIZATION

but technically the cyclization (before the second amination) can be done in any amount h2o

...and maybe safer to just do in water and re x to acetylate in alcohol

If water added you get 4-acetyl DET

If no water you will yield more 5-acetyl

Yield will be 50-50 split at 50% vol water.

~~~====~~~~~~==========\/\\\\\////\/==========~~~~~~====~~~

~~~====~~~~~~==========\/\/\/ \/\/\/==========~~~~~~====~~~

~~~~====~~~~~~======HARDER!TO F!!CK!UP======~~~~~~====~~~~

~~~===~~~(5-(EtO/AcO)-DET/DEAMT)(4-(EtO/AcO)-DEAMT)~~~===~~

~~~====~~~~~~==========/\(impure)/\==========~~~~~~====~~~

~~~====~~~~~~==========@@(better)@@@==========~~~~~~====~~~

~~~====~~~~~~==========\/\\\\\////\/==========~~~~~~====~~~

~~~====~~~~~~==========*^#^*^#*^#*^#==========~~~~~~====~~~

DIETHYL 4/5 ACETOXY/ETHOXY

TRYPTAMINE/ ALPHAMETHYLTRYPTAMINE

Ingredients:

witch hazel added to iron out powder (25-75 metabisulfite and sulfite of sodium) with ammonium chloride forms ammonium ethylsulfide

AKA ammonium thioethane

MELATONIN -> tryptamines

TRYPTOPHAN -> alphamethyl tryptamines

you basically just add 2M of this to l-tryptophan+HCl OR melatonin after dissolve additional 2M Ammonium Chloride added to 100% alcohol(methanol(best), ethanol, propanol but NOT Isopropyl):

(IF TRYPTOPHAN 3M NaH(CO3)2), so 3mol:3mol acid, for 4/5 Ethoxy or

(IF TRYPTOPHAN 2M NaH(CO3)2 plus 0.5M MgCO3), so 2:0.5:3mol acid(not considering amino acid).

---------OR:-----

(IF MELATONIN 3Mol K or NaH(CO3)2) so 3mol:3mol acid for Ethoxy or

(IF MELATONIN 1.5Mol Ca/MgSO4 or Ca/MgCO3) for 3:3mol (ion pairs)->Cl- .

Sulfates and transition metal bi phosphates should work fine but ive only tried with magnesium, calcium or sodium.

AS WRITTEN: if you want to form ethoxy groups instead of acetyl use an alkali hydrogen carbonate instead of earth alkali carbonate, sodium hydrogen bicarbonate 0.5mol and then use MgCO3 0.333mol and this will...:

to recap,

ethanol best solvent the best fit alcohol for the scale and geometry of the adduct alcohol, so MeOH-DMT EtOH-DET PrOH-DPT

witch hazel ingredients:

MIX

ethanol 10-25% + 75-90% H2O,

WITH

0.06-0.12 g/mL dry tannic acids, polyphenol powders or (esp. volatile polyphenols!!!), MUST BE ADDED TO THE ETHANOL AND H2O

(or just use a witch hazel solution or ethanol and skip forming this mixture)

. if no reducing polyphenols, use pure R-OH alcohol(EtOH)/

mixture:

witch hazel solution:

-mix approx ~=0.08g/mL tannins/polyphenol - 0.1666M ethanol solution. Make 300mL exactly.

-use 14% witch hazel from a pharmacy.

Obtain 300mL of either of the two acceptable titrations here.

(reducing polyphenols are important to save one addition of acetic acid, which will drop your yield from melatonin to 1/2 and tryptophan to 1/6).

-form na/ca/k/mg Cl/F/Br2 from approx. 1M of any of these individual salts in WITCH HAZEL 150mL. (pure volatile , radical polyphenols (optional) with (NECESSARY) 1/6 mol ETHANOL with from Mg/Na/K/Ca SO4/PO4

(prefer sulfate vs phosphate anytime here, can split yield)

-form a separate reducing phenol+ethanol mixture as our 'witch hazel the same way as you did before.

-add 0.5M (1/2 Mol) Melatonin or Tryptophan to the separate 150ml witch hazel mixture (now flask #2)

-Add 4M Ammonium Chloride to the mixture with sulfates in witch hazel 150ml flask #1

-------

Allow the ammonium chloride solution both at most 5-10 minutes of stirring to finish thioalkium (NH4SC2H5) formation.

-------

NOW, POUR AND CONTIOUSLY STIR THE TWO MIXTURES TOGETHER IN A 300mL flask. flask#3

-------

!!!!!REFLUX THE WITCH HAZEL/ SULFATE / AMMONIA / ETHANYL SOLUTION IN A HOT WATER BATH, AND STIR!!!!!

WATCH THE PRECIPITATION FOR ANY CRUDE CONDENSATE AND CONTINUE TO MIX THE SOLN UNTIL DRY

!!! HOWDY HOLA WHULA !!!

you should precipitate 100% pure 5-(EtO/AcO)-(DET/DEAMT) and or 4-(EtO/AcO)-(DET/DEAMT) sulfates.

with 1-2M chlorides of table salts

as the condensations finish.

uh you get ammonium acetate somewhere tho

.....................

Hello,

Here below is my synthesis I have been using to produce 5F-ADB, a synthetic cannabinoid

Reagents: Indazole-3-carboxylic acid (cas 4498-67-3) 100 g; Methanol (MeOH) 2500 ml; Sulphuric acid conc. (H2SO4) 100 ml 98%; Ethyl acetate (EtOAc) 7500 ml; Sodium bicarbonate aqueous solution (NaHCO3) 1000 ml; Distilled water (H2O) ~8000 ml; Sodium chloride (NaCl) ~300 g; Magnesium sulphate (MgSO4); Tetrahydrofuran (THF) 1000 ml; Potassium tert-butoxide (t-BuOK) 70 g 1-Bromopentane 80 ml; Sodium hydroxide 1M aqueous solution (NaOH) 600 ml; Hydrochloric acid 1M aq. solution (HCl); Dimethylformamide (DMF) 1000 ml; EDC (cas 1892-57-5) 82 g; BuOH (cas 71-36-3) 58 g; DIPEA ( cas 7087-68-5) 180 g; L-valinamide (cas 4540-60-7) 100 g; Stage 1 Methyl 1H-indazole-3-carboxylate

1. Indazole-3-carboxylic acid 100 g solution in MeOH 1500 ml and 5 l round bottom flask is treated with concentrated H2SO4 100 ml (98%).
2. The mixture is refluxed for 4 h.
3. After that, the mixture is concentrated with vacuum and dissolved in ethyl acetate (EtOAc) 2500 ml.
4. An organic phase is washed with saturated sodium bicarbonate aqueous solution (NaHCO3) 1000 ml, H2O 1000 ml and brine 1000 ml. Then, the mixture is dried over magnesium sulphate (MgSO4).
5. Ethyl acetate (EtOAc) solvent is evaporated under reduced pressure. Methyl 1H-Indazole-3-carboxylate 83 g is obtained as a white solid.

Stage 2 Methyl 1-pentyl-1H-indazole-3-carboxylate

1. To a cooled Methyl 1H-Indazole-3-carboxylate 100 g, 0 °C solution in THF 1000 ml t-BuOK 70 g is added.
2. The mixture is warmed to a room temperature, stirred for 1 h and cooled to 0 °C. 1-Bromopentane 80 ml is added dropwise with a constant stirring.
3. The mixture is warmed to a room temperature, stirred for 48 h and distilled water 1000 mL is added.
4. Layers are separated. An aqueous layer is extracted with EtOAc 2x500 ml. Combined organic phase is washed with distilled water 3x500 ml and brine 1000 ml. Then, Organic solution is dried over MgSO4.
5. Solvent is evaporated under reduced pressure. Amethyl 1-pentyl-1H-indazole-3-carboxylate clear glass-lik

Now, the issue I am running into is I want to start developing the precursor myself and synthesizing that as well. I just am unclear on what compounds go into the specific precursor I need.

The compound is

Methyl (S)-2-(1H-indazole-3-carboxamido)-3,3-dimethylbutanoate

Case number:

cas# 2709672-58-0

Any idea on what the precursors may be or how I could go about figuring that out? Thanks

Hi I’m looking to piece together a full working understanding of what goes into a 2c x synthesis as well as the relation between 2c b fly and nbomes. I notice 2c b fly is not in pihkal tihkal.

Separately, can anyone point me towards resources looking into the “smart pill” era info. Eg erox “nexus”. I’m very excited about strong nootropic action let’s say.

I want to introduce a pentyl group to 5-ethylbarbituric acid.

I would like the sodium salt.

Could I deprotonate with NaOH in DMF and add 1-bromopentane to introduce the pentyl group at the 5 position? So I have both a pentyl group and ethyl group at the 5 position?

Thanks in advance, and apologies for any misunderstandings, I'm still learning.

Hello fellow and aspiring bees! I am currently a student in organic chemistry 2, and we have an upcoming 3 week project which aims to isolate and verify any natural organic compound of our choosing. The only catch is no alcohol, nicotine, or controlled substances. With that in mind I was wanting to see if you guys had any ideas as to what could be interesting, but not too challenging. Ultimately the grade is heavily based on a purity of 95% or greater so it is something to keep in mind. First compound that came to my mind was scopolamine from the nightshade family, and a quick search shows that an isolation is possible via liquid extraction. What do you guys think would be a good idea, or should I stick with something simpler or less controversial?

Just like the title says , got the some crazy idea and I would like to hear what other thinks of it. Anyway, we all know that mixing amphetamine and pregabalin can lead to overdose or pshycotic episodes, but mayde it could be controled somehow . Insane idea is really my wonder what would happened if you take pregabalin,which haves acidic properties and amphetamine base and make their salt.

Of course there are historical reasons - The Hive was probably an inspiration to us all and showcases how incredible cooperation can be in chemistry. A single bee is doomed to die.

The whole swarm can achieve incredible feats.

But this doesn't speak to people who don't feel nostalgic towards the old, HTML, outdated forums.

So instead I'll simply point towards what we have accomplished over the last few years:

• We optimized the Henry reaction for pretty much every aldehyde. Ethanolamine has become the gold standard. [LINK]

• We optimized the reduction step via borohydride-copper to yield pretty much every phenethylamine in over 80% yield. [LINK]

• We developed and optimized use of NaDCC for synthesis of MDA from helionamide. We also pioneered the best, reflux-free, one-pot synthesis of helionamide from helional. No more nickel fuckery. [LINK]

• We developed the synthesis of chlorinated analogs of mescaline, total synthesis of muscimol, optimized, in-depth synthesis of ketamine by various routes, syntheses of MMDA and DMMDA, BDB, 2C-H, 2C-I, 2C-B, 2C-C, DOM, moclobemide, methylphenidate, GBL and GHB by various routes, DMT by various routes, optimized decarboxylation of tryptophan to perfection. There is too much of this to link.

• We developed the one-pot pathway from helional to MDP2P by a couple methods, including ones applicable to >500g and are on our way to make it completely OTC. [LINK]

• We developed a wonderful protocol for enantiopure dextroamphetamine and levoamphetamine utilizing OTC reagents [LINK]

• We developed the synthesis of P2P from cyprinal [LINK, LINK]

• We have a thread full of real-life photos of reagents, intermediates and products. [LINK]

I think you guys get the point. People on the Vespiary are dope as fuck. And the catch is... you're not invited just to lurk and read. You are also invited to ask stupid questions, propose ideas, learn the basics (and also the advanced nuances). You are invited to run experiments. To share failures, not just successes. To share photos of your compounds. To share the music you like (yeah, we really have a thread for that). To troubleshoot. To make your own lab equipment. To learn to purify reagents and solvents. To read references. To ask for references you can't access.

You don't even have to have a real e-mail address to register. Seriously.

The only thing we require is the will to learn and the will to share what you've learned. Don't be afraid to post a little introduction about your motives and interests.

It's a community after all, for fucks sake. Not just a database.

See you soon, I hope?

Why is all the write ups be useing nickel acetate as their choice for the Beckman for aldoxime to amide. When you can use sulfuric acid with water and reflux. Why would one use xylene and nickel acetate at 150c over lower Temps and sulfuric acid? https://www.sciencedirect.com/science/article/abs/pii/S0009261416304985 https://pubs.acs.org/doi/10.1021/jo01153a018 Edit I added on an old one I just looked thro in old chem book I add and it said something about it as well. I. So confused why it's not being used when it's super common and apparently high yield. I'm guessing maybe there is a reason... hoping some one with a actual degree can chime in..

Edit: upon further research I forgot that aldoxime doing a standard Beckman makes nitrile's and ketoxime creates amides. All other points that have been mentioned are extremely valid and accurate. But the major reason is if you did a standard Beckman you wouldn't come out with a amide it would be a nitrile. Now I'm surprised it hasn't be better explained is the Beckman being inployed here is not a standard Beckman because using the nickel acetate the aldoxime forms a nitirle and in the first part of the reaction and then continues on in a secondhand part of the reaction to form the amide! That is the major reason. Along with everything that is mentioned. But even I'd tou could get a standard Beckman to work you would have a nitirl not a amide! Hope that makes sense I literally spent 5+ hrs studying and first thing you will find is aldoxime- Beckman= nitrile and ketoxime-Beckman=amide. So this is on fact a 2 part Beckman reaction. I could go into the whole explanation on how it first forms a nitril thwn foes on to form a amide but honestly I'd have to explain the whole reaction and I really don't want to. But Google Beckman and you will see what I'm saying is absolutely factual!

Reading through it shows that I need a pretty standard high seed money of about 250 dollars. I can get the glassware, scales, and stirplate, but the hard thing for me is DCM, that shit is expensive and hard to get, is that really the only thing I could use? not to mention there are many other ingredients that dont seem to be necessary in some recipes, like sodium nitrite, which is similarly hard to get, but really easy to just synthesize from my understanding

Vespiary has been down for a few days now for me. Anyone know what's up?

The Scripps Research Institute submitted a patent a few years ago, but for the life of me, I cannot find it.

Any help is greatly appreciated.

Wet Product

Synthesis of 2-haloacetamido-benzophenone:

To a pressure-proof glass tube, 1mmol of substituted 2-amino/methylamino-benzophenone of choice and 3mL NMP is added. Stir until all solid dissolved, heat can be applied if needed. To the solution, 1.2mmol of haloacetyl halide is added at RT (all bromoacetyl bromide, chloroacetyl chloride or bromoacetyl chloride will work). The reaction is started upon contact, indicated by evolution of HCl/HBr gas and the change of color of the solution. The mixture is set aside for 30min.

Synthesis of benzodiazepine:

To the mixture from previous step, 2mL more NMP is added. The reaction is quenched by pouring 3mL of water with 1mmol Na2CO3 dissolved. A lot white solid was parcipitated out with evolution of CO2 gas. 1mL of 40% HMTA solution and 2.2mmol of NH4OAc is then added. The tube is sealed and put into a hot water bath at 65C for 3-4h. After completion or reaction, the solution was slowly poured into ice water allowing product to be parcipitate out, followed by simple filtration with coffee filter and washed multiple times with ice water until no NMP can be smelled. The product is dried in air for 24h and ready to be used.

Edit: For 2-amino derivatives, it is better to keep the solution cool in order to prevent forming of byproduct; For 2-methylamino derivatives, it may be necessary to heat up the solution before addition of haloacetyl halides due to lower reactivity.