Reduction of Ephedrine to Methamphetamine Using Hypophosphorus Acid[ Back to the Chemistry Archive ] Hypophosphorus Acid & Sodium Hypophosphite HandbookPreparation of Hypophosphorus AcidPreparation of Sodium Hypophosphite (Brit. Pat. 803179) 115g of white phosphorous is emulsified and reacted with aqueous NaOH to obtain 270g NaH2PO2.H2O (70%). Preparation of aqueous sodium hypophosphite (Jap. Pat. 58185412) White phosphorus is dispersed together with slaked lime used as an assistant in an aqueous medium by stirring in an inert gas atmosphere under heating at or above the melting point of white phosphorus. The dispersion is mixed with a solution of caustic soda under heating and stirring to effect the reaction of the components. The product is separated into solid and liquid, and the mother liquor is added with a phosphate donor such as phosphoric acid. When the phosphate donor is phosphoric acid, its amount is about 0.6mol per 1mol of dissolved calcium, and the pH of the system is maintained usually to about 8-11. The reaction is carried out at about 50-100°C, and the reaction product is aged for about 30min. The Ca(II) dissolved in the mother liquid is precipitated in the form of calcium apatite, and the high-purity aqueous solution of sodium hypophosphite can be recovered by this process. Hypophosphorous acid purification Free hypophosphorous acid, H3PO2, is prepared by acidifying aqueous solutions of hypophosphite ions, H2PO2-. For example, the solution remaining when phosphine is prepared from the reaction of white phosphorus and a base contains the H2PO2- ion. If barium hydroxide, Ba(OH)2, is used as the base and the solution is acidified with sulfuric acid, barium sulfate, precipitates and an aqueous solution of hypophosphorous acid results. Ba2+ + 2 H2PO2- + 2 H3O+ + SO42- => BaSO4 + 2 H3PO2 + 2 H2O The pure acid cannot be isolated merely by evaporating the water, however, because of the easy oxidation of the hypophosphorous acid to phosphoric acids (and elemental phosphorus) and its disproportionation to phosphine and phosphorous acid. The pure acid can be obtained by extraction of its aqueous solution by diethyl ether. Pure hypophosphorous acid forms white crystals that melt at 26.5° C. The electronic structure of hypophosphorous acid is such that it has only one hydrogen atom bound to oxygen, and thus it is a monoprotic oxyacid. It is a weak acid and forms only one series of salts, the hypophosphites. Hydrated sodium hypophosphite, NaH2PO2×H2O, is used as an industrial reducing agent, particularly for the electroless plating of nickel onto metals and nonmetals. Hypophosphorous acid from sodium hypophosphite To a stirred solution of 717.8 g of a 32% hydrochloric acid solution in a 3-necked 2 liter flask was added 615.42 g of powdered sodium hypophosphite. The temperature of the solution rose about 2° C. Water was removed from the stirred reaction mixture by reduced pressure distillation at a temperature of about 55°C ±7° C at a pressure of 44-72 mmHg until a hypophosphorous acid concentration of about 80 wt% was obtained. After cooling to room temperature, sodium chloride that had precipitated was filtered from the reaction mixture. The filter cake was washed twice with 32 wt % hydrochloric acid. The recovered product contained 355.7 g of hypophosphorous acid. The analysis showed that the product contained 0.9 wt% sodium, 3.2 wt% chloride, and 80.96 wt% hypophosphorus acid. Chloride ion was removed from hypophosphorous acid using an ion-exchange column (height 221/4", diameter 11/8"). The column was packed with Rohm and Haas Resin IRA-410 in the chloride form and was regenerated using 5% NaOH. The results from using this column at different H3PO2 and Cl- concentrations are shown below.
Ephedrine Reduction to Methamphetamine with Hypophosphorus Acid and IodineBy Wizard X I would recommend a large excess of reducing agent for quick reduction. Charge flask with 100 ml (0.1Lt) of 50% H3PO2 (0.965 mole H3PO2 per 100 ml) fit reflux condenser, add 3x33 grams (99 grams, 0.39 mole) portions of I2 while cooling in ice bath down the reflux condenser[1]. After addition of I2, gently heat so HI gas is evolving from the condenser, add 5 mls potions of H2O down the condenser till HI gas stops evolving and hence maximum amount of HI saturation kept in solution is acheived. Now add 50.4 g (0.25 mole) of ephedrine hydrochloride and boil under reflux for at least 2 hours, let cool and then made basic with 20 % sodium hydroxide solution (20 grams NaOH in 100 mls H2O) in ice bath to liberate the free base. Set-up glassware for steam distillation and steam distil until the distillate is almost neutral to litmus.[2] The libertated freebase methamphetamine which seperates is solvent extracted with three, 50-75 ml ether (or toluene) portions and the ether/amine solution is first washed with 50 mls of distilled water and the ether/amine solution dried with anhydrous sodium carbonate.[3] After removal of the ether (or toluene), the oil was vacuum distilled at a vacuum of 15 mmHg at 93°C. The yield is 80 - 82%[4]. Notes:
Ephedrine ReductionMajor reduction reaction: C6H5-(CHOH)-CH(NHCH3)-CH3 + HI =====> C6H5-(CHI)-CH(NHCH3)-CH3 + H2O C6H5-(CHI)-CH(NHCH3)-CH3 + HI =====> C6H5-CH2-CH(NHCH3)-CH3 + I2 Minor reduction reaction: C6H5-(CHI)-CH(NHCH3)-CH3 + H3PO2 + H2O =====> C6H5-CH2-CH(NHCH3)-CH3 + H3PO3 + HI Ratio of ephedrine to HI is theoretically 1:2, however a 1:3 is used for better reduction and yeild. Hypophosphorus to HI CalculationsH3PO2 + H2O + I2 ==>> H3PO3 + 2HI Hypophosphorous 50% w/w. F.W = 66 g/mol. Density = 1.274 g/ml. 100mls (0.1Lt) of Hypophosphorous 50% w/w contains: (1.274 / 50)/100 = 0.637 g/ml H3PO2 = 0.00965 mol/ml H3PO2. 0.00965 mol/ml H3PO2 x 100 = 0.965 mol/100ml H3PO2. OR (0.637/66) x 1000 = 9.65 moles H3PO2 per 1000 mls. (mol/Lt) Since we use 100mls (0.1Lt), then 9.65 x 0.1 = 0.965 mol/100ml H3PO2. Now since the ratio of Ephedrine : HI is 1:3 = (3/1), we require 0.75 moles of HI for every 0.25 moles of ephedrine hydrochloride. Since we have 0.965 mol of H3PO2 and 0.39 moles of I2 (99/253.8 = 0.39), then the ratio of I2:HI is 1:2 = (2/1); so 0.39 moles of I2 reacts with the Hypophosphorous acid to form 0.39 x 2 = 0.78 moles of HI. Finally, the excess Hypophosphorous acid, H3PO2 is 0.965-0.39 = 0.575 moles of H3PO2 is excess. The ratio for H3PO2 : I2 is 1:1, so only 0.39 moles of H3PO2 is needed to react with 0.39 moles of I2 to form 0.78 moles of HI. Not only do we have enough HI; 0.78 moles to reduce 0.25 moles of ephedrine hydrochloride, but a large excess of 0.575 moles of H3PO2. Alternatively, Charge a 1000ml flask with 100 ml (0.1Lt) of 50% H3PO2 (0.965 mole H3PO2 per 100 ml), 100 mls of distilled water, fit reflux condenser, add 4x49.5 grams (198 grams, 0.78 mole) portions of I2 while cooling in ice bath down the reflux condenser[1]. After addition of I2, gently heat so HI gas is evolving from the condenser, add 10 mls potions of H2O down the condenser till HI gas stops evolving and hence maximum amount of HI saturation kept in solution is acheived. Now add 100.8 g (0.5 mole) of ephedrine hydrochloride and boil under reflux for at least 2 hours, let cool and then made basic with 20 % sodium hydroxide solution (20 grams NaOH in 100 mls H2O) in ice bath to liberate the free base. Set-up glassware for steam distillation and steam distil until the distillate is almost neutral to litmus.[2] Since we have 0.965 mol of H3PO2 and 0.78 moles of I2 (198/253.8 = 0.78), then the ratio of I2 : HI is 1: 2 = (2/1); so 0.78 moles of I2 reacts with the Hypophosphorous acid to form 0.78 x 2 = 1.56 moles of HI. Finally, the excess hypophosphorus acid, H3PO2 is 0.965-0.78 = 0.185 moles of H3PO2 is excess. The ratio for H3PO2 : I2 is 1:1, so only 0.78 moles of H3PO2 is needed to react with 0.78 moles of I2 to form 1.56 moles of HI. Not only do we have enough HI; 1.56 moles to reduce 0.5 moles of ephedrine hydrochloride, but an excess of 0.185 moles of H3PO2. P-fed Reduction to Methamphetamine with Hypophosphorus Acid and IodineBy Pebble Assuming that you have extracted P-fed from your pills, you are now ready to convert the p-fed to methamphetamine. The structure of P-fed is so closly related to methamphetamine, that people have learned to alter it's structure in order to convert it to methamphetamine. What one is actually doing is reducing a benzylic alcohol. In our case, it appears as OH in P-fed. So, we strip this off completly and throw on an additional H (Hydrogen) to the p-fed. So, by removing the OH and adding a H we have thus altered the structure and have created methamphetamine. This is for small-scale reduction of P-fed to methamphetamine. If one wanted to make meth in the range of ounces, etc. I would not reccomend one cook in an open container. Fire or explosion are at a much higher risk when cooking anything above 10 grams using this procedure. This is why the Push/Pull apparatus is so popular. No, fumes, smell, and IT CAN reduce the risk of injury if something does go wrong. Notice I said IT CAN. There is no fool-proof method of safety when working with chemicals of this nature, unless proper lab equipment, etc are used; and this still does not elimanate the dangers, just reduces the probability that an accident will happen. If one wanted to have 5 grams as their finished peoduct, than 6-8 grams of P-fed. Some can get 90% yield where others may only get 35% yield. This takes time to perfect, but results will vary WITH YOU. Take your 8 grams of p-fed and put this into a 250ml. flask or pyrex meassuring cup. Slowing add Iodine crystals unto the p-fed is mixed well with the iodine. You don't want it very purple, just enough iodine to where all the white is no longer visible. Remember, you mix the iodine and the P-fed up as you go along, you just don't throw it in and go from there. O.K., a good way to meassure your Hypophosphorus acid is to use a ratio of 1ml. for every gram of P-fed that you are using. 50% or 30% Hypophosphorus will work, but you might want to add more Hypophosphorus acid if it was 30%. I have seen "LAB GRADE 30%" act no different than 50%. So, you make the call, just do the math to equal out the 30-50 ratio if using 30% Hypo. O.K. put in you Hypo. Doesn't take much. Take your cooking vessal and move around slowly to mix the acid with your I2 and P-fed. You'll notice that the contents will start to liquify. It will look red, so agitate the cooking vessel until it turns yellow. After it has turned yellow, place on heat. You can use gas or electric on this small cook. If using a electric eye, place an iron skillet or something over the eye. Usually Med heat to High will be O.K., you might have to experiment to see what works best. You don't want it to get to hot, so remove give it a couple of swirrls. Place back on and leave on heat, repeating this a couple of time if neccessary. When it befins to boil, let it, for about 10 sec. and remove and let it sit, DO NOT SHAKE. You will notice that it just keeps boiling. It may do this for 30 sec. or more and then quit. This is your first major reaction. Take a little wiff of the smoke, you'll notice that it'll take your breath away. Don't worry about dying from this, it's O.K., just smells bad. Agitate it a few times and crank up the heat a little. Remember, don't let it get to hot, but don't let it cool down either. When it begins to boil a second time, remove it after about 10 sec. and let it sit. After you remove it from the heat, it will continue to get faster and faster and really smoke. This is your second major reaction and this is what does the conversion of your P-fed to methamphetamine. If you removed it a second time and it hardly did anything. Than try again to ensure that it converts. If you take another wiff you should notice that the smell is bearable now, and actually quite pleasant in some cases. There are about three distinct smell that let you know it converted. If you pay attention in the beginning to the smell, you notice the difference and it's very noticable. Keep agaitating and letting it sit, maybe place on heat source for a few secs. and remove and agitate. It's done, but it should go to a golden or yellow looking oil. Or it may go very clear looking with only a touch of yellow. Or if it turns green or is dark this is O.K. Sometimes this happens with the use of H2O2. As long as no particles or floating around. Let it cool down at this point. The whole reaction should have lasted no longer than about 10-20 min. After the cooking vessal is WARM to the touch add colemans and lye and the lye wash. If it got to hot and is like caemel syrup on the bottom, a piece of wood can be used to mix the dope up to get to going. If you don't stir up the contents in a situation like this, your lye will never push your dope up into the coleman lyer. Also, if your lye begins to go into your coleman layer, a little alcohol around the edges and a few drops in the middle will keep it down. After the wash, draw up your coleman fuel layer, for some it turns purple. The lye should have been added until the p.h. read +13. Next, put the coleman/dope layer into a 20 0z. coke bottle and add an equal amount of distilled water. Use HCL to gas the coleman/dope layer so that the HCl will push the dope into the water. It all in there when the P.H. of the water reaches around 7. Stopping around +8 is safer than trying to go to 7. Turn the bottle over and lossen the cap until the water begins to fall into the evaporating dish. Make sure no coleman gets through. Now, just evoparate the dish with the water/dope and there you go! If done correctly, you could have a 90% yield, but for many and new beginners the yield is usually around 35-40%. There are many tricks and little secrets that are involved that one can possess and learn as they do this. As for as quality, I dreamed of one line and it was so good I broke out into a sweat instantly. It has no bad comedown effects like I have expericed with the "Nazi Method" and doesn't cause sore muscles, etc. It's a fast and easy method for anyone wanting to aquaire a few grams of meth. for bigger quantities, cooking will be necessary, but everything else will remain the same. |