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MDMB-4en-PINACA Synthesis

  1. 2024-05-24 at 3:45 PM UTC
    #1
    kratomslave Yung Blood
    This is my third attempt at this synthesis. Every time I have ended up with an oily type
    Liquid and that has not crystallized. My
    Main precursor and base of the reaction is MDMB-INACA (which is getting harder and harder to obtain as Chinese suppliers have stopped producing).

    I see varying reaction temperatures, ranging from 60-80°C, along with varying reaction times, ranging from 2-5 hours total stirring at these heats.
    Does anybody know what the ideal conditions are for this reaction?
    Potassium carbonate is highly insoluble in DMF, at least at room temperature (lit says solubility is 7.5g of K2CO3 per 1000ml of DMF at 25c), but I’ve also noticed from performing many ADB-BUTINACA syntheses, that much of the k2co3 remains undissolved throughout the reaction even at 80-90°C
    The adbb syntheses seem to work just fine without K2CO3 being completely dissolved.
    I just thought yield could be improved if K2CO3 was fully dissolved in the solution but perhaps it's not necessary
    Wouldn’t the dissolution of k2co3 only not matter if it was simply acting as a scavenger, which if I’m not mistaken is not the primary function of k2co3 in this reaction?
    I see varying ranges for the amounts of solvent (2-3L DMF), amounts of 5-bromo (465g-515g), and amounts of k2co3 (700g-856g)
    using equimolar amounts of MDMB-INACA and 5-bromo-1-pentene should indicate the use of about 515g 5-bromo per kg MDMB-INACA (apprx. 3.5mol) — should I be using a molar excess of 5-bromo, an excess of MDMB-INACA, or is equimolar fine?
    should I be leaning more towards 2 or 3 liters of DMF?
    will a heavy excess of k2co3 affect the reaction? 700g is already a significant molar excess (apprx. 5.2mol), I know excess will enhance the reaction rate by providing more hydroxide ions, but what about the possibility of competing elimination reactions or altering the regioselectivity of the reaction?
    Will water mess up the reaction? Is using anhydrous k2co3 / DMF very important?
    I’ve seen some have issues with crystallization of the final product, only being able to obtain oily residues when using ice water for the final crystallization step straight from the reaction mixture (method 1, seen in my write-up below), as opposed to extracting twice with DCM, concentrating to dryness under vacuum, & recrystallizing from anhydrous ethanol (method 2) — has anyone here been able to obtain solid product from the first method? (procedures described in my write-up below)
    I’m aware that many Chinese labs have stopped producing the main ingredient MDMB-INACA, though the vendor I’m working with seems to offer it although they won’t give any IUPAC name or Cas no. for it. Is it likely that they are actually selling me a completely different precursor than MDMB-INACA that still works to produce a noid with this procedure?
    Another user has told me "You are right that reacting it with 5-bromo-1-pentene yields 5cl, impossible to crystallize, and I have reported having reacted the same precursor with 1-bromo-5-fluoropentane and obtaining a stronger product, and I presume it is 1971007-89-2, the S- isomer (or possibly racemic mixture)”
    my question is, would replacement of 5-bromo-1-pentene with 1-bromo-5-fluoropentane not yield 5F-MDMB-PICA? (this is what a Chinese vendor told me)

    Anyone with experience regarding the synthesis of noids would be helpful. I can’t manage to yield high quality crystals and not this fucking oily bullshit.
  2. 2024-05-24 at 4:15 PM UTC
    #2
    Buff Billy African Astronaut
    This is a pretty cool method, I've never heard of this before
  3. 2024-05-24 at 4:40 PM UTC
    #3
    kratomslave Yung Blood
    Originally posted by Buff Billy This is a pretty cool method, I've never heard of this before

    Years of trial and error trying to yield indazole3carboxamides and pyrazole based syncans.
  4. 2024-05-24 at 5:12 PM UTC
    #4
    Buff Billy African Astronaut
    Originally posted by Croutonslave Years of trial and error trying to yield indazole3carboxamides and pyrazole based syncans.

    Have you heard of the vespiary? It's a Chem forum and I think they would be able to help you better than anyone here.
  5. 2024-05-24 at 6:50 PM UTC
    #5
    kratomslave Yung Blood
    Originally posted by Buff Billy Have you heard of the vespiary? It's a Chem forum and I think they would be able to help you better than anyone here.

    Yea but hasn’t helped much. I have posted on several forum pages looking for help but haven’t got much. Very little information around these new gen noids. Older ones (JWH and AM series) are a lot easier to find synthesis information on. I’ve had so much trouble with these new gen noids that are ultra potent and get unstable due to the lack of information of them. It’s crazy how much the spice game has changed. Been around and fooling with synthetics since the days of euphoric knowledge. Ah man the good ole days.
    The following users say it would be alright if the author of this post didn't die in a fire!
  6. 2024-05-24 at 7:05 PM UTC
    #6
    Buff Billy African Astronaut
    Yeah this is the first time I'm hearing of it. I figure most "research chems" aren't widely made in the civilized world because it's usually some multi stage bullshit with very little literature besides old patents written by REAL PROFESSIONALS. The Asians are much more suited to making this shit.

    I read that they sell "chemistry kits" of the exact chemicals you mentioned, that's funny as hell. I wouldn't trust those shifty Chinese at all. I don't know how you would be able to tell MDMB-INACA apart from something similar, I found a MSDS for MDMB-5Br-INACA but that has even less info

    I can't even find what it's melting point is. It doesn't sound very stable according to this, maybe they sold you expired product.
    Cas No. 2709672-58-0 SDF
    Synonyms Methyl (S)-2-(1H-indazole-3-carboxamido)-3,3-dimethylbutanoate
    Canonical SMILES O=C(N[C@H](C(OC)=O)C(C)(C)C)C1=NNC2=C1C=CC=C2
    Formula C15H19N3O3 M.Wt 289.3
    Solubility DMF: 12.5 mg/ml; DMF:PBS(pH 7.2)(1:1): 0.5 mg/ml; DMSO: 10 mg/ml; Ethanol: 3 mg/ml Storage -20°C
    General tips Please select the appropriate solvent to prepare the stock solution according to the solubility of the product in different solvents; once the solution is prepared, please store it in separate packages to avoid product failure caused by repeated freezing and thawing.Storage method and period of the stock solution: When stored at -80°C, please use it within 6 months; when stored at -20°C, please use it within 1 month.
    To increase solubility, heat the tube to 37°C and then oscillate in an ultrasonic bath for some time.
    Shipping Condition Evaluation sample solution: shipped with blue ice. All other sizes available: with RT, or with Blue Ice upon request.
  7. 2024-05-24 at 8:24 PM UTC
    #7
    kratomslave Yung Blood
    Originally posted by Buff Billy Yeah this is the first time I'm hearing of it. I figure most "research chems" aren't widely made in the civilized world because it's usually some multi stage bullshit with very little literature besides old patents written by REAL PROFESSIONALS. The Asians are much more suited to making this shit.

    I read that they sell "chemistry kits" of the exact chemicals you mentioned, that's funny as hell. I wouldn't trust those shifty Chinese at all. I don't know how you would be able to tell MDMB-INACA apart from something similar, I found a MSDS for MDMB-5Br-INACA but that has even less info

    I can't even find what it's melting point is. It doesn't sound very stable according to this, maybe they sold you expired product.

    It’s a possibility that either the precursor is expired, or that it isn’t actually MDMB-INACA and it’s some other crazy noid precursor thats yielding an entirely different product. I’m gonna run GCMS on my last batch to see if I get a match with anything in CAS system. Ya never know, I might have just made something brand new with this reaction lmfao.
  8. 2024-05-24 at 8:38 PM UTC
    #8
    Bradley Florida Man
    Originally posted by Croutonslave Yea but hasn’t helped much. I have posted on several forum pages looking for help but haven’t got much. Very little information around these new gen noids. Older ones (JWH and AM series) are a lot easier to find synthesis information on. I’ve had so much trouble with these new gen noids that are ultra potent and get unstable due to the lack of information of them. It’s crazy how much the spice game has changed. Been around and fooling with synthetics since the days of euphoric knowledge. Ah man the good ole days.

    I was on EU as well.
  9. 2024-05-24 at 11:02 PM UTC
    #9
    kratomslave Yung Blood
    Originally posted by Bradley I was on EU as well.

    Fuck bathsalts man. Killed the party for everyone. I remember being jacked up on some bullshit pentylone tweaking out when I read that the feds had ek compromised. Nuked all my hard drives. Lost so much information but I like to think I saved some jail time.
  10. 2024-05-25 at 1:06 AM UTC
    #10
    Buff Billy African Astronaut
    Originally posted by Croutonslave I’m gonna run GCMS on my last batch to see if I get a match with anything in CAS system. Ya never know, I might have just made something brand new with this reaction lmfao.

    That seems to be the only way. You can find GCMS charts for this stuff but no melting points. Maybe i'm just old fashioned and nobody uses melting points anymore.

    This is the only place i've seen online that does original research for this class of compounds but i'm still not totally convinced they aren't cops.

    https://bbgate.com/
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