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And to the object that made this possible - the Internet. This is for theoretical argument only. In no way do I condone this activity. This is a hypothetical synthesis for: The synthesis as described 1. The synthesis itself can be performed in a series of weekends or in a straight shot. Be prepared to read and learn. Read the whole thing before you start. This list is the basics. Set up for a vacuum distillation like on page 53 of Zubrick. Put one of your mL 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. Start turning up the heat slowly! Whatever temp it starts to come over at - make a note of it. 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. 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. 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. In your mL RBFlask: Set up for distillation not vacuum. In the distillation flask your mL RBFlask put: Remember to turn on the water in the condenser! We are removing methylal, and methylformate from the reaction contents and therefore driving the reaction to the right - or getting more of what we want. After four hours and while the solution is still hot, set up to vacuum distill IE its already set-up - now just add the vacuum hose! Turn up the heat. Crystals should start to form in several minutes. Filter off these Ammonium Chloride Crystals. Now set up for distillation of the remaining liquid again - Add a couple more boiling stones. Distill off half of the remaining liquid. At some point the whole mass will crystallize into a yellow-white solid. This is fine for the next step. It may be a little wet, but if you let it crystallize hot spontaneously in the flask with heat it should be fairly dry. Seal it in a wide mouth jar until needed. As a way to check your product - if you live in a relatively humid area, you can put a crystal of your product on the table - walk away - and when you come back a small puddle of water will be on the table where your product was. Another way is to put 20mL of water in a cup then add 5g of the NaOH to it. If you do the same with Ammonium Chloride, it will just smell like ammonia. This can be stored at room temperature, forever. HCl with excellent results. Paraformaldehyde is the polymerized form of formaldehyde - but unlike most polymerization processes - this one is reversible - so Paraformaldehyde and formaldehyde can be interchanged at will. This step has been called the Wacker Oxidation. It uses PdCl 2 as a catalyst to put and oxygen across a double bond. If you do this correctly, you will have more MDMA. HCl than you know what to do with. After the addition, the solution was dark reddish orange. Make sure the stir bar is spinning - Now - Walk away. This reaction requires NO additional heating! The oil fell out of solution to the bottom. This is when its nice to have a Big Sep Funnel. Now we need to define several things. The upper layer in this case! After you flood the reaction contents shake the container to mix the solution, give it about 10 minutes to settle - two layers will form. The upper aqueous layer was decanted from the oil IE it was poured off. Keep the DCM washes - They contain the goods. You now should have about mL total of DCM washes. Pour the DCM washes and the Organic layer together. This will remove the other reaction by-product - hydroquinone. The NaOH layer Aqueous: Put several boiling stones in too. Set up for vacuum distillation. Now remember when we distilled the safrole? What temp did it come over for you? Start your vacuum distillation by first turning on your vacuum - if you remembered your boiling stones, then it will begin to boil immediately. This is the DCM coming off first. You are going to have to change the flask, when the temp gets to above the safrole temp. This is a bit tricky, because you are going to have to release the vacuum. Start the vacuum immediately, but be careful here, because the Organic layer that you are distilling might jump out of the flask and into the receiving flask - so if you can - vary the vacuum so that the vacuum comes on GRADUALLY! IE with an aspirator, turn on the water slowly. Re-weigh the flask for your yield calculation - you should have over g of ketone. With an aspirator you can vary the vacuum when you are turning it on. You simply turn on the water slowly. IE Increase water pressure slowly. Look at how it refracts light. It will become a very viscous liquid. Total waste of effort, time, and precursors. The ketone is unstable. And then it will be useless. At room temp, it will rearrange in about a week - depending on where you live - if you keep it in the freezer - it can last months - FREEZER! After its in the freezer you can stop for today. This process utilizes the electronegative properties of the Aluminum. This is the oxidized form of Aluminum. We will remove this part of the foil so that the aluminum can reduce the imine with elemental Al. This reaction actually has two parts. This reaction reacts the ketone with methyl-amine to form an imine - water is produced as a product. Second, the imine is reduced Hydrogen is added across the double bond to the amine. Set up your stand and clamp so that, when the flask is clamped to the stand the bottom of the flask is about 4 inches 10cm from the table top. This is so that you can put the heating plate and stirbar combo under it. Have your thermometer already in its thermometer adapter so you can throw it in the flask at any second. Prepare the following, put them in a jar and have them ready at a moments notice: It is very important that these are ready before you start! Amalgamation was allowed to proceed until there was the evolution of fine bubbles the formation of a light grey precipitate, and the appearance of occasional silvery spots on the surface of the aluminum. This should take between 15 and 30 minutes. When amalgamation is complete, pour out the water into the milk jug. Pour it out into the jug. So basically, you wash the Al pieces with 2xmL of water. Dump out as much of the water as you can in 10 seconds or so - then immediately go to the next step - leave the Al foil in. This will remove most of the Hg from the solution. If you let the Al squares sit in between washes, they will heat up and re-form the Al 2 O 3 in a matter of seconds. So be quick and have the ingredients ready for the procedure. Put the thermometer in the solution. Start being very paranoid about the temperature. Stirring is necessary so, with the heat off, stirbar on, flask sitting in the cool water bath. The whole time you are doing this the contents are a grey sludge. Remember to keep the stirbar going! If the stirbar is difficult to start going. This reaction should go no less than 6 hours. Now, after you are convinced that the reaction has stopped 6 hours later - IE the temp of the solution is room temperature, and there is no more foil chips in the mix. Stir the contents some more, and then let the stirbar stop and then let the solution rest for at least 30 minutes. The NaOH solution will make that grey sludge into a filterable consistency. Then in a matter of minutes the whole thing will be resting on the bottom of your flask. The reaction contents will settle out. The grey sludge will settle to the bottom, and a clear yellow liquid will rise to the top. Pour off the clear yellow liquid. Pour off the 2nd clear yellow liquid once it settles. Add the 2nd clear yellow liquid to the first. Do this several times, or until the clear liquid is no longer yellow. This is an extraction out of the reaction contents. The more you do this process, the higher your yield. After you have gotten as much of the yellow liquid out as you could. Put the grey sludge in the same milk jug waste container. Dispose of it properly - the milk jug contains elemental Hg - Not a lot - less than 0. But you should dispose of it properly. Not down the sink. Set up for vacuum distillation Boiling Stones! Make sure you get the alcohol out. When the alcohol is close to being gone - the solution might spontaneously separate in your distillation flask. Not to worry - the top layer is probably your product, and the bottom is water. This works very well for our target molecule, and any molecule that contains an amino group. Stir or shake it up. A lot of the brown oil should go into the acid solution. Now pour into this solution 30mL of DCM. Shake again and let it settle. You will notice two layers formed - The top layer is the Aqueous layer - which contains your product, and the bottom layer contains the DCM, polymerized crap, and non Nitrogen containing molecules. Pour off the top layer That contains your product and discard the DCM layer. Note that the aqueous layer contains the product - Do not discard the aqueous layer! You can discard the DCM washes, because they contain nothing useful what-so-ever. When you do this the Aqueous layer will turn a milky white and may heat up just a little bit. A light brown oil will fall out of the solution. This is your product in the freebase form. Shake and let it settle out. Pour off the top Aqueous layer, and keep the DCM this time! The DCM washes contain the goods! Wash the aqueous layer twice more with 50mL of DCM. Combine those DCM washes that contain your product, and continue. That should be good enough. You should have a light brown oil in the flask - it kind of looks like thick Newcastle Beer. This must be done in anhydrous conditions. If its not, then you will not get crystals. If water is present, then you can expect to get crapola. This first step can be done ahead of time. Like, during a distillation or reaction: There might be a little heat evolution, but not to worry Shake it up and then let it sit till the MgSO4 settles out. Now shake the bottle and let it sit for 15 minutes. You must do this at least three times - It really is much better to do it four times - Why fuck it up now right? You can actually do this while you are distilling or waiting for a reaction to proceed. Pour it into the flask that contains the MDMA oil, and drop the stirbar in too. Stir so that the whole thing is mixed up real well - Now drip in Muriatic Acid slowly. Test with pH paper every 5 drops or so - keep adding the Muriatic Acid until the pH of the solution is - or just barely acidic. Set up for vacuum distillation, and distill the solution, distill this with the stirbar in instead of the boiling stones - IE When the solution has reached a pH of - Start distilling. Stir the crystals to promote even heating. The crystals will be a brown-yellow color. The brown-acetone is poured off, and the acetone wash is repeated. After the acetone wash, dry the crystals. You should have around 15g of dry crystals. And these crystals are ready for consumption. For me at least. If you have completed this, congrats. Now Teach Someone Else! If you do - we WIN! This file is a part of the Rhodium site archive. This Aug static snapshot is hosted by Erowid as of May and is not being updated. A must, throughout this text, pages from this book will be mentioned. These are the best. Trust me its worth it for holding the glassware to the stand - these support several hundred dollars in glass - buy a nice one! But aspirators are cheap Boiling Stones for distillations. Small shards from a broken coffee mug Tubing about 10ft. Zip-Strip furniture polish remover Hg salt 1 gram of: WEIGH the receiving flask! Write the weight on a piece of tape and tape it to the flask! Step 6 2 hours work 6.
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