MDMA Recrystallization

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Topic author: theficus Subject: MDMA Recrystallization Posted on: Apr 25 2006 12:25:23 PM Message: -----BEGIN PGP SIGNED MESSAGE----Hash: SHA1 is assessing various methods of MDMA recrystallization and is leaning towards the following method. would like some input from those who have recrystallied MDMA. Is this a good method? Are the directions accurate? Is there a better or easier method? Quote: Once you have your dry drug hydrochloride salt crystals, sometimes you want to get them more pure, because impurities can be trapped inside the tiny clumps of crystals. A good way of doing this is to recrystallize. The idea behind this is to find a solvent that the crystals are kind of soluble in and kind of not. Alcohols usually work well for this. When talking about solvents and solid materials, hot solvent dissolves more solid than cold solvent, so this can be used to your advantage. (The case is opposite for gases but I won't go into that). Get two containers. Put some alcohol in one and bring it up to boiling. Put your crystals in the other container. Slowly add boiling alcohol to your crystals and they will dissolve. Use just enough alcohol to dissolve all of your crystals. Now since cold alcohol doesn't dissolve crystals very well, cool down the alcohol/product and the crystals will come back out (recrystallize). The slower you cool the alcohol, the bigger the crystals are. The bigger the crystals are, the fewer impurities will be trapped inside of them, and the purer your product will be. So big crystals = pure crystals (usually). One good way for ensuring that your alcohol cools down nice and slow is to put some water in a pot and heat it to boiling and take it off of the heat. Then put your container with hot alcohol/dissolved crystals in the pot of water being sure not to get any water into the alcohol, cover the container, and let it cool down to room temperature. Then you can put the container with alcohol in the refridgerator to cool more. Then into the

freezer to cool more. Then you can filter your pretty crystals out. Now there is usually still a little bit of product left in the alcohol, so if you boil off say 75% of the alcohol and repeat the cooling process you can get some more crystals. There are other ways of changing the solubility of the crystals in the alcohol, such as adding acetone or ether to the alcohol, but the temperature method works quite well, is cheap, and simple. So newbies should use it first, then experiment with other methods if they want to.

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Replies:
Reply author: ChesireCat Replied on: Apr 25 2006 12:37:22 PM Message: Isopropyl alcohol works great using the method described...I have seen pictures left attached to my litterbox of solid crystals the the diameter of a quarter and nearly 1/2 inch in thickness.

Reply author: theficus Replied on: Apr 25 2006 4:03:24 PM Message: -----BEGIN PGP SIGNED MESSAGE----Hash: SHA1 Does 91% Isopropyl Alcohol work well or should Isopropyl Alcohol? -----BEGIN PGP SIGNATURE----Version: PGP Desktop 9.0.5 - Enterprise license iQA/AwUBRE6rRO2NUwCsRvmjEQI+CgCaArVTwRJh+Sfb6ifQAxgCOAPgZsgAn0aY 2lT816iLUJw1ZMvF6oQPc/vu =mI2e -----END PGP SIGNATURE----aim for pure

Reply author: ChesireCat Replied on: Apr 25 2006 5:56:40 PM Message: The hatter uses 99% . but it really doesnt matter much. just anticipate waiting longer for the crystals...

Reply author: TaurineMonster Replied on: Apr 25 2006 6:48:44 PM Message: any water present will disolve mdma.

Reply author: getspunhvfun Replied on: Apr 28 2006 12:41:39 PM Message: recrystalization in 100% DH2O works for MA

Reply author: mad_chem Replied on: Apr 29 2006 08:04:23 AM Message: Recrystallization of MDMA using IPA/ACETONE ALL solvents should be Anhydrous Dissolve product in a minimum quantity of boiling anhydrous Isopropyl Alcohol (IPA) When all product has gone into solution add 4 times the amount of freezer chilled anhydrous acetone to the solution. Example: 75ml of IPA dissolves 20-25g of product you will add 300ml of freezer chilled anhydrous acetone. Seal and put in freezer for 1 to 8 hours Filter out crystals using a buchner funnel. Air dry crystals. Low heat source can be used. Macerate crystal to make sure there is no solvent trapped in crystal lattice NOTE: Acetone is dried using Anhydrous MgSo4. Add 20g MgSO4 per liter of solvent. IPA can be dried using CaO. *** Also Acetonitrile is supposed to be very good at recrystallizing MDMA

but I have never tried it. I remember bees at the hive who swore by it. Never the less the method outlined at the top works extremely well and gives beautiful crystals, trust me.

Reply author: ChesireCat Replied on: Apr 29 2006 08:51:06 AM Message: I wish the hatter had an ass like that :> He'd be much easier to look at!

Reply author: hell fire Replied on: Apr 30 2006 01:41:24 AM Message: Anhydrous acetone is by far the best for recrystalising. Gives such a nice clean product. Store bought acetone is roughly 99% - 99.95%. Any dessicant can be used to dry the tone to 100%. Add some dessicant to the 99% and syphen off the top layer.

Reply author: mad_chem Replied on: Apr 30 2006 09:29:32 AM Message: First of all you cant use any desiccant with acetone Second, you can't just assume that hardware store acetone is 99.5% pure. Third, if youre making MDMA you should have vacuum filtration which is what you should be using to remove the desiccant. People who use turkey basters are just lazy. 4th Acetone is not the best solvent because its the only one you have used. The recrystalization process I outlined works better then just acetone. And by the way, have you tried a recrystalization with Acetonitrile?

Reply author: myhero Replied on: May 01 2006 10:32:10 AM Message: What SWIM knows is that acetone is dessicated with K2CO3.

Reply author: ChesireCat Replied on: May 01 2006 11:10:17 AM Message: Actually vacuum filtration is not preffered for removing dessicant.. see zubrick

Reply author: mad_chem Replied on: May 02 2006 11:45:35 AM Message: myhero you're right, anhydrous potassium carbonate can be used in the place of magnisium sulfate to dry acetone but to my knowledge Mg2SO4 is much easier to come by (epsom salts) and it will absorbe more water then the later as Mg2SO4 forms a heptahydrate while K2CO3 only forms a dihydrate. Sodium and calsium sulfate can also be used for acetone by the way. As for IPA anhydrous potassium carbonate, anhydrous magnisium and calcium sulfate, and quick lime can be used. Chesirecat you're right too, Zubrick does state that, but i have used vacuum filtration with a medium whatman filter paper with excellent results. I guess if you want to go by the book you can use gravity filtration with a fluted filter paper or use a pipette to remove the top layer (but its easy to disturbe the bottom powder layer).Also when your working with larger volumes of solvents the later methodes can be time consuming.

Reply author: hell fire Replied on: May 02 2006 12:52:44 PM Message: Quote: Originally posted by mad_chem First of all you cant use any desiccant with acetone Second, you can't just assume that hardware store acetone is 99.5% pure. Third, if youre making MDMA you should have vacuum filtration which is what you should be using to remove the desiccant. People who use turkey basters are just lazy. 4th Acetone is not the best solvent because its the only one you have used. The recrystalization process I outlined works better then just acetone.

And by the way, have you tried a recrystalization with Acetonitrile?

SWIHF knows the acetone you get OTC from HW shops or as a paint thinner is between 99% and 99.95%. Acetone is also widely available in NV remover at arround 50%, the rest being H2O and other crap. The NV remover can be distilled to yeild 99% - 99.5% then it will have to dessicated to get anhydrous acetone. And no it's not the only solvent swihf uses. SWIHF should have spoken more clearly. Most dessicants can be added to acetone the rest can be used in a dessicator. SWIHF uses alot of acetone, it's cheap, works for most things and smells good too. Anhydrous acetone works perfectly for recrystallizing MDMA to me that just looks like a waste of IPA, time and money. Reply author: mad_chem Replied on: May 03 2006 6:34:13 PM Message: Bro I'm just discussing for the sake of discussing but there you go needing to defend yourself. I just want to put in my 2 cents of experiance I'm just adding to the pot for others who might want to experiment and expand there knowledge. Personally I find using a dual solvent crystalization work better by making larger crystals which have a more precise melting point (They melt over the spand of a degree insted of sevral.) The more info and experimental data there is out there the better it is for evry one.

Reply author: wetundies Replied on: May 04 2006 11:29:31 AM Message: lol, what a silly thread. Everyone is claiming that "their" solvent system is the best to use when recrystalizing MD compounds. Why can't it just be said that there are numerous solvents that are able to achieve this goal? I don't think any one of the above are any better than the each other. Each have their good qualities. If you have patience and dont mind the time it takes to make your 99% ISO anhydrous then that would be a good route. Bare in mind that 1% of 99% is H20 and guess how much MD-whatever can dissolve in 10ml of H20!! Thats money right there. This holds true for acetone, as store purchased acetone is never anhydrous. Never ever ever. Methanol works great, is cheap and easy to obtain but once again, needs to be made anhydrous before SWIWU will even consider using it to recrystalize whatever. All are good, and as the first post mentioned, alcohols are usually the easiest ones to prepare and use.

Reply author: C_C_C Replied on: May 04 2006 11:34:20 AM Message: Another true story is that each solven system has its own properties which will make the one solvent system better for removing the unwanted compound X while another is better to remove compound Y therefor one should try probably to use two dual solvent recrystallisations to get where one wants to get... So far

Reply author: wetundies Replied on: May 04 2006 11:39:51 AM Message: Good point methlab. One impurity may be more susceptible to dilution in one solvent than another. Generally, the impurities in most mdma made from the common methods, Al/Hg/NaBH4 reduction, are common impurities found in the workup, or "washes" of the non polar solvents that contain the freebase. Sodium Bicarb, Sodium Chloride, Magnesium Sulfate. Drying agents, etc. This has been confirmed by mass spectral interpretation.

Reply author: i8an8th Replied on: Aug 04 2006 9:03:58 PM Message: How well would some ACS grade 95% ethonal alchol work? Instead of the IPA..

Reply author: ChesireCat Replied on: Aug 11 2006 05:13:23 AM Message: Hard to say EXACTLY without consulting the merck.. BTW. some cat is pissed drunk and to high to find this bible.. your on your own.. lol...

Reply author: i8an8th Replied on: Sep 06 2006 8:45:57 PM Message: Swim would like to see some before and after photos..

Reply author: ChesireCat Replied on: Oct 23 2007 10:29:46 PM Message:

Quote: Originally posted by i8an8th Swim would like to see some before and after photos..

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after (sorry the pics are not to scale)Attached Image: