08-12-03 18:39
No 453211
Would anyone who owns a copy of SOMM care to type down the first few paragraphs of the chapter "Reductive Alkylation Without The Bomb", Method One? Swim would like to know what % NaOH solution, and the amount, is introduced into the reaction flask before the reagents. Thank you.
(Chief Bee)
08-12-03 20:12
No 453224
(Rated as: excellent)
Here is an old OCR... But you really should be using this instead: ../rhodium /p2p-met
Reductive Alkylation Without The Bomb (from SOMM III)
The process of reductive alkylation using the hydrogenation bomb, as you saw in the previous chapter, is not without difficulties or dangers. Just for starters, consider the danger of hydrogen gas building up in a poorly ventilated workplace. Add to that the danger of the bomb blowing up if the welding of the seams is not done well. Also think about the hassle involved in making enough Raney nickel to produce multi-kilos of methamphetamine. The last problem can be minimized by reusing the Raney nickel used in the previous batch. In this way, the underground chemist can get away with adding only half as much fresh nickel as would otherwise be added, but he must be doing one batch right after another to keep it fresh.
All of these problems, except for the hydrogen gas danger, can be eliminated if he is able to get his hands on activated aluminum turnings. In this method, the aluminum turnings take the place of hydrogen gas as the catalyst in the reductive alkylation process. The yields are very good, the process is very simple, and no special equipment is required. The reaction is also quick enough that it can be used in large-scale production.
Activated aluminum is next to impossible to purchase, but very easy to make. The raw material is aluminum foil. The foil is amalgamated with mercury by using mercury chloride. The result is aluminum amalgam.
To make activated aluminum, the chemist takes 100 grams of the aluminum foil, and cuts it into strips about 2Yz cm wide, and 15 cm long. He folds them loosely, and puts them into a 3000 ml glass beaker or similar container. He does not stuff them down the neck of the flask or similar container from whence they would be hasslesome to retrieve. He packs them down lightly so that they are evenly arranged, then covers them with a .1% solution (1 gram in one liter of water) by weight solution of sodium hydroxide.
He warms the mixture by setting it into a hot water bath until a vigorous bubbling of hydrogen gas has taken place for a few minutes. He is careful here that the mixture does not overflow! Then he pours off all the sodium hydroxide solution as quickly as possible, and rinses the strips with distilled water, and then with 190 proof vodka. This preliminary treatment leaves an exceedingly clean surface on the foil for amalgamating with mercury.
While the surface of the strips is still moist with vodka, he adds enough of a 2% by weight solution of mercury(II)chloride (aka mercuric chloride, HgCl2) in distilled water to completely cover the foil. He allows this to react for about 2 minutes, then pours off the mercury solution. He rinses off the strips with distilled water, then with 190 proof vodka, and finally with moist ether. Moist ether is either purchased as is, or made by adding water to anhydrous ether with stirring until a water layer begins to appear at the bottom of the ether. The chemist uses this material immediately after making it.
Method 1
In this method, the activated aluminum turnings react with alcohol to produce hydrogen gas. This hydrogen then reduces the Schiff's base formed from methylamine and phenylacetone to give methamphetamine.
The chemist needs a magnetic stirrer-ho/plate to do this reaction. On top of the stirrer-hotplate, he places a Pyrex bowl or cake dish large enough to hold a 3000 ml flask. The bowl or dish cannot be made of metal, because the magnetic stirrer will not work through it.
He places the 3000 ml flask in the dish and fills it with cooking oil until the oil reaches about halfway up the sides of the flask. He must be sure to leave enough room for the oil to expand as it heats up. He puts the magnetic stirring bar in the flask along with 1600 ml of absolute alcohol or 190 proof grain alcohol. Then he adds 340 ml of phenylacetone and 450 ml of 40% methylamine in water. Now he turns on the magnetic stirrer and begins heating the oil in the dish. He keeps track of the temperature of the oil with a thermometer, and does not allow it to go above 100øC. While the oil is heating up, he adds 180 grams of activated aluminum turnings to the flask. He makes sure that the stirring is fast enough that the turnings do not settle to the bottom of the flask. The reaction mixture will quickly begin to turn grey and foamy. The aluminum is added at such a rate, the bubbling and foaminess it produces does not overflow the flask. When all of it has been added, a condenser is fitted to the flask, and water flow is begun through it.
The chemist now lets them react for 8 hours. He keeps the temperature of the oil bath at 100øC, and the stirring strong. The activated aluminum slowly dissolves and produces hydrogen gas. The explosive danger from this gas is eliminated by running a length of tubing from the top of the condenser out the window.
When the 8 hours are up, he removes the flask from the oil bath and wipes the oil off the outside of the flask. He filters the solution to remove the aluminum sludge, then rinses the sludge with some more alcohol to remove the last traces of product from it. The rinse alcohol is added to the rest of the filtered product.
The underground chemist can now distill the product. He pours it in a 3000 ml round bottom flask that is clean and reasonably dry, and adds a few small pieces of pumice. He places the flask on the electric buffet range, then sets up the glassware for fractional distillation, as shown in Chapter 3. He begins heating it. The first thing that distills is a mixture of alcohol, water, and methylamine. This occurs when the temperature shown on the thermometer is about 78-80°C. He collects about 1600 ml of this mixture, then removes the flask from the heat. He lets it cool down, then pours the contents of the 3000 ml flask into a 1000 ml flask, along with a few fresh boiling chips. He puts about 15 ml of alcohol in the 3000 ml flask. swirls it around to dissolve the product left clinging to the insides, then pours it into the 1000 flask.
The chemist again sets up the glassware for fractional distillation, with a 250 ml flask as his receiver. He applies a vacuum, preferably from an aspirator, and begins vacuum distillation. When the boiling gets under control, he begins heating the flask. The last remnants of alcohol and water will soon be gone, and the temperature shown on the thermometer will climb. When it reaches about 80øC with an aspirator, or about 70øC with a vacuum pump, he quickly changes the receiving flask to a clean, dry 500 ml flask, and reapplies the vacuum. He will get about 350 ml of clear to pale yellow methamphetamine free base. A few milliliters of tar will be left in the distilling flask. The liquid free base is converted to crystals by dissolving it in ether or benzene and bubbling dry HC1 through it, as described in Chapter 5.
The underground chemist gets an even purer product by varying this procedure slightly. Once the 1600 ml of alcohol, water, and methylamine is distilled off, he pours a mixture of 650 ml of 28% hardware store variety hydrochloric acid and 650 ml of water into what remains in the 3000 ml flask, after it has cooled down. A lot of heat is produced in the mixing because the methamphetamine free base is reacting to make the hydrochloride. So he adds it slowly, then swirls it. When it has cooled down, he stoppers the 3000 ml flask with a cork or glass stopper and shakes it vigorously for 3 to 5 minutes. It should pretty much all dissolve in the hydrochloric acid solution. Now he adds 200 ml of ether or benzene to the flask and shakes it up well. The ether or benzene dissolves any unreacted phenylacetone and tar. He lets it sit for a few minutes. The ether and benzene layer floats to the top. He pours it slowly into a 1000 ml sep funnel, so that the top layer all gets into the sep funnel. Now he lets it set, then drains the lower acid layer back into the 3000 ml flask.
The acid must now be neutralized to give back amphetamine free base, so it can be distilled. The chemist mixes up a solution of 350 grams of lye in 400 ml of water. When it has cooled down, he pours it slowly into the acid solution in the 3000 ml flask. A lot of heat is generated from the reaction. When it has cooled down, he stoppers the flask and shakes it strongly for about 5 minutes. When standing, the amphetamine forms a layer on top. He slowly pours it into a 1000 ml sep funnel. He drains the water layer back into the 3000 ml flask. The methamphetamine layer in the sep funnel may have some salt crystals floating around in it. He adds 100 ml of benzene to it plus a couple hundred ml of a dilute lye solution. He stoppers and shakes the mixture. The salt will now be dissolved in the water. He drains the water layer into the 3000 ml flask and pours the methamphetamine-benzene solution into a clean 1000 ml flask. There is still some methamphetamine left in the 3000 ml flask, so he adds a couple hundred ml of benzene to it. If there is a lot of undissolved salt in the flask, he adds some more water to it. Now he shakes the flask to dissolve the meth in the benzene, then lets it set. The benzene comes up to the top. He pours it off into the sep funnel, and drains off the water layer. He pours the benzene layer into the 1000 ml flask with the rest of the product.
He can now begin distilling it. He adds a few boiling chips, sets up for fractional distillation, and proceeds as described in Chapter 5. The yield once again is about 350 ml of free base, which makes close to 400 grams of pure crystal.
(Stranger)
08-12-03 22:26
No 453242
Upon thorough reading of both write-ups, can you or anyone please explain why the methods on Rhodiums page are preferable over Uncle Fester's method? (aside from the much higher fondness that bees have toward Rhodimu then Uncle Fester). Thank you for all your help!
(Stranger)
08-12-03 23:22
No 453261
If you want your very own copy of SOMM (I assume it's a full copy), along with some other potentially interesting stuff (lots of explosives-related items, if that's an area of interest, although some other drug-related books such as "Psychedelic Chemistry" by Michael Valentine Smith and UF's "Practical LSD Manufacture"), check this link out:
http://swi.1av10.nu/dist/
The files are zips, the ones I downloaded contained a small picture of the cover of the book (if applicable), an ID file and the text in Word format.
I'm totally unsure where I found this link, so it's entirely possible that it's been posted before, but I did run a few searches before writing this and they came up with nothing.
(Stranger)
08-17-03 18:49
No 454236
Rhodium,
Thank you for your prompt response to my post; it helped me out a great deal and while I read the methods described at ../rhodium /p2p-met
"The residue was taken up in 1000ml water, acidified by the addition of conc HCl, and washed with 3x50ml DCM, basified with 25% NaOH, and extracted with 3x100ml DCM."
My 2 questions are:
1 - Since no amount of conc HCl and 25% NaOH were specified, does that mean any reasonable amount will suffice?
2 - Is conc HCl the same as 37% HCl in water?
Thank you.
-xSpikeHead
(Chief Bee)
08-18-03 04:08
No 454331
1 - Since no amount of conc HCl and 25% NaOH were specified, does that mean any reasonable amount will suffice?
Absolutely not. It means that you should enough acid or base to make the solution distinctly acidic (pH ~1-3) or distinctly basic (pH ~11-13). To see if you have reached the desired pH range, you use standard universal pH paper or equivalent.
2 - Is conc HCl the same as 37% HCl in water?
Yes.