Sunteți pe pagina 1din 1

Procedure Dissolve 4.

0g Nickel Chloride hydrate (light green crystals) in 75 ml 95% ethano l w/ mag stirring and warming to 50C. After salt is dissolved remove stir bar and add 1ml water and 1ml conc. HCl.1 While solution at 50C slowly add 5g regular Re ynolds wrap torn up into 0.25 x 1.0in strips in 1g portions with manual stirring . The aluminum will SLOWLY react with the nickel salt forming the metal Ni(s) th rough metathesis as a dark grey chunky powder which settles to the bottom. A gen tle effervescence of hydrogen occurs during reaction. Add aluminum at a rate tha t maintains a steady effervescence and keeps temperature roughly in the 50C range . Note this may take up to two hours! At the end of Al addition all green color from nickel salt should be discharged. If any color remains add another gram of aluminum and wait for soln to clear. Precipitated Nickel powder was added to 100 ml 20% NaOH soln and manually stirred at 60C for 30 min. Excess NaOH is decanted and nickel is washed with 5 x100ml aliquots of distilled water to remove excess base. At this point Urishubara nickel catalyst is prepared and ready for reducti on. Dissolve 5g pure phenylnitropropene in 50ml Ethanol and add to Ni solution.2 Now slowly add 3ml conc. HCl3 and 1 gram shredded aluminum w/ manual stirring. Alum inum will slowly dissolve with a more vigorous effervescence of hydrogen than th e first step. Maintaining good stirring with a glass stirring rod is essential i n beginning. Attempted magnetic stirring will result in frustration because nick el is ferromagnetic and will stick to stirbar preventing surface area exposure n ecessary for reduction. After aluminum is dissolved add three more milliliters H Cl and one more gram Al. Repeat adding acid and Al until 10 grams Al and about 3 0ml HCl has been added. Aluminum reacts slowly. Expect addition to take about si x hours, longer if temp falls below 50C. Constant stirring towards end is not nec essary, just give mix a good stir occasionally. After all aluminum is added and mostly decomposed slowly pour in a soln of 30g N aOH in 100ml H2O with careful stirring. Wear goggles and be careful! Base neutra lization is highly exothermic! In 30 minutes all aluminum sludge will solvate in to bottom aqueous layer and a nice orange alcohol layer reeking of amine will se ttle out on top. Nickel is not dissolved by the NaOH so it will remain floating around between the two layers but this does not present a major problem. After a ll, it s not poisonous like mercury or anything! Now decant off the top orange org anic layer and distill off alcohol down to a orange stinky syrup completely diff erent smelling than the P2NP. Dissolve these goodies in acetone and slowly add s ulfuric acid to precipitate the amine sulfate. Voila!!!!!! about 3 grams light y ellow amphetamine sulfate. Notes Addition of water and acid found to be necessary to initiate rxn between NiC l2 and Al. When nitropropene was added to NiCl2 soln before conversion to Ni powder was complete some polymerization occurred greatly reducing yield. It seems essentia l to add P2NP to rxn after Ni is fully precipitated. Use of Sulfuric acid produced inferior results causing polymerization of P2N P to red tar. Increasing Yield: Use overhead mechanical stirring to keep nickel catalyst bette r suspended during reduction. Re-extract aqueous NaOH/Al layer w/ toluene and wo rk up in standard manner. Use larger amount of nickel catalyst and more aluminum for H2 generation.