A Complete MDMA Synthesis for the First Time Chemist 1

Discussion in 'Drug Chemistry' started by ancient powers, Aug 1, 2007.

  1. ancient powers

    ancient powers Member

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    A Complete MDMA Synthesis for the First Time Chemist

    Introduction

    Thanks to Strike, Rhodium, Ritter, Osmium, r2d3, Semtex Enigma, Spiceboy, ChemHack, Labrat, Eleusis, Ketone/LabGrrrl, and a personal hero, Dr. Shulgin. And to the object that made this possible - the Internet.

    Disclaimer: This is for theoretical argument only. IF someone chooses to follow this synthesis, note that the product has been 'Scheduled 1' by the United States Government, and offenders can be prosecuted. In no way do I condone this activity.

    This is a hypothetical synthesis for: 3,4-methylenedioxy-N-methylamphetamine. Or MDMA.HCl. Or Ecstacy. The synthesis as described 1. does not put off nasty fumes, 2. requires suspicious chemicals, and therefore is 3. perfect for the clandestine chemist. The synthesis itself can be performed in a series of weekends or in a straight shot. If one were to follow this exactly - with no shortcuts - buying everything they're told - doing exactly what is written - they and they're friends will have a lovely spring. For those who think they are better than the instructions as written - be prepared to screw it up at least 4 times before success (or you finally figure out I'm right). Be prepared to invest ~$800. Be prepared to read and learn. It's also a good idea when investing in chemicals to buy 5x what is needed for a synthesis - this way you can repeat it without buying it again. Read the whole thing before you start. There is some prep-work that can be done ahead of time, or while you're distilling. Good luck.

    Overview:

    1. Distillation: of Natural Oil to obtain pure Safrole

    2. Rxn: Formaldehyde + Ammonium Chloride -> MethylAmine.HCl (MeAm.HCl)

    3. Rxn: Safrole -(Wacker Oxidation(PdCl2+Benzoquinone))-> MDP2P

    4. Distillation: of Reaction contents to yield pure MDP2P

    5. Rxn: MDP2P -(Al/Hg Amalgam (MeAm.HCl) -> MDMA oil

    6. Crystallization: (MDMA oil + HCl in IPA/Xylene) (anhydrous conditions)

    What you need:

    This list is the basics. Do not even start this without ALL the Chemicals and Apparatus.

    Apparatus and Glass:

    · 'The Organic Chemistry Lab Survival Manual' by James W. Zubrick. (A must, throughout this text, pages from this book will be mentioned. ~32$) (and very handy pictures of glass set-ups)

    · Distillation Apparatus(1x500mL and 1x1000mL Round Bottom Flask, 1x250mL Round Bottom Flask, condenser, distillation adapter, vacuum adapter, thermometer adapter) (Get Ground Glass Joints. These are the best. 19/22 or 24/40 - my first set was 19/22 - and is still used to this day.)

    · Thermometer (0°C to ~300°C)

    · Stand (Home Depot - (2x10in., flange, 2 ft. of ½in pipe))

    · Clamp (Buy it. Trust me its worth it) (for holding the glassware to the stand - these support several hundred dollars in glass - buy a nice one!)

    · Hotplate/Stirrer combo (got to have it, its worth it) (www.labx.com - spend $200)

    · Magnetic stir bar (look on the Web) (teflon coated)

    · Water Aspirator (or a good vacuum source. But aspirators are cheap <$20)

    · Boiling Stones (for distillations. Small shards from a broken coffee mug)

    · Tubing (about 10ft. total (3 meters) - hardware store - vacuum tubing is better than dialysis tubing - but both will work)

    · Vaseline (not much - for coating of the ground glass joints)

    · Measuring Cups (Prefably pyrex, and in milliliters (mL))

    · 10 various sized glass containers/bottles (250mL, 500mL, 1L, 2L etc)

    · Scale (a three beam analytical balance are great - and can be found for less than $100 - www.balances.com - they can weigh as much as a kilo and as little as 0.1g - perfect!)

    · pH paper (chemical supply) (just one roll will do - ~10$) (nothing specific, just need to tell the difference between an acid and a basic solution)

    Chemicals:

    · Safrole (160g)(sassafras oil, yellow camphor oil) (Natural/Essential Oil distributor)

    · Dimethylformamide (DMF) (350mL) (Diethylformamide or Formamide will work)

    · p-Benzoquinone (Quinone, Benzoquinone) (120g) (Photo Shop, or Chem supply)

    · Palladium Chloride (PdCl2) (2g) (Photo Shop, or chem supply)

    · Methylene Chloride (DiChloroMethane, DCM) (this can be distilled from automotive solvents (just go into Nationwise, PepBoys, Sears, AutoZone And read the labels) Or a Liter can be bought from a Chem supplier.)(Zip-Strip furniture polish remover)

    · Hg-salt (1 gram of: HgCl2, Hg(NO3)2, Hg(acetate)2, HgCl, It can be anything, and 1g should last you a long time.)

    · Isopropyl Alcohol (IPA, Pharmacies 91% Isopropyl Alcohol will be available)(get +3L)(don't get the 70% stuff) (or you can get pure stuff from a chem supplier)

    · Epsom Salts (Magnesium Sulphate) (MgSO4) (grocery store/pharmacy) (Spread out on a cookie sheet, and bake in the oven at 200°C for 3hr to dry them - pretty useless if you don't dry it)

    · Thick Al foil (heavy duty, or pie pans from the Grocery store)

    · Muriatic Acid (31.45% HCl)(Pool pH down, Driveway cleaner, ~3$/gallon)

    · Sodium Hydroxide (NaOH) (Drain Cleaner Crystals) (Read these labels, Get the stuff that is JUST NaOH.) (Red Devil Lye, Lye - Hardware Store)

    · Ammonium Chloride (NH4Cl) (Photo Store or Chem Supplier)

    · Paraformaldehyde (Hardware store) (called Mildewcyde or DiGas - made by the same people who brought you Damp-Rid - hint-hint)

    · Peanut oil (this is a high boiling oil that we will use as an oil bath on the hotplate/stirring plate combo)

    · Acetone (for cleaning your glass and crystal work-up) (Paint Section of Hardware Stores)

    · Xylene (for crystallization) (paint section - thinner - get it specifically)

    1. Distillation: of Natural Oil to obtain pure Safrole.

    A Comprehensive Description of this Step by Chromic

    Set up for a vacuum distillation like on page 53 of Zubrick. Always put a little Vaseline on the ground glass joints - this way they won't stick when you try to take them apart. Put as much Natural oil (Sassy, Camphor, ect) as you have, but not more than 300mL, into the 500mL Round Bottom Flask (RBF) with several Boiling Stones. Put one of your 250mL RB flasks as the receiving flask. Set up your Water Aspirator Vacuum, in the sink (this may require setting this up a day before - parts, trips to the plumbing store, etc.) and attach the vacuum hose to the aspirator and then to the vacuum adapter on the distillation set up. Start turning up the heat slowly! SLOWLY! The slower you do it, the better/purer your safrole will be. At normal pressure safrole boils at 232°C - but under your vacuum, it may boil at anywhere from 110-160°C. Whatever temp it starts to come over at - make a note of it. And if the temp is higher than 160°C - check your seals on the tubing and glassware - More than likely there is a little leak. Remember that Vaseline! At the end of the distillation, you should have a water white oil that really refracts light - And has a lovely smell - a little like potpourri.

    Distillation set-up: Set up the distillation set-up on your bed, before you try to put it together on the stand. You will get a good idea about how the pieces go together, and become familiar with the fragility of the whole thing. Read Zubrick for advise about where to place the clamp.

    The Peanut Oil: A bowl with a flat bottom rests on the Hotplate. It is filled with Peanut Oil. The distillation flask sits in the bowl but not touching the bottom, so that the Hotplate heats the bowl, the bowl heats the Peanut Oil, the Peanut Oil heats the distillation flask. This is VERY effective. And will be perfect for all your distillation needs - especially if you do it under vacuum.
     
  2. branflakes

    branflakes Member

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    Safrole is a List I chemical, buddy. Are you suggesting to grow sassafras?
     
  3. kidsmoke

    kidsmoke Member

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    Not only that, but this synthesis is far from "complete."
     
  4. branflakes

    branflakes Member

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    Maybe that's because it's only Part 1?
     
  5. Intense.Reaction

    Intense.Reaction Member

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    yeh wheres the rest of it? oO
     
  6. Intense.Reaction

    Intense.Reaction Member

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    ignore previous post lol
     

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