Its in chapter 7 as well. Oh fuck it, here it is:
Aluminum Amalgam Reduction[43]
72.5g of aluminum foil is cut into one inch squares and placed into a 3000ml erlenmeyer flask or other suitable glass container. A solution of 1.8 grams of mercuric chloride (HgCl2) in 2530 ml water is added, and the mixture is stirred occasionally over 30 minutes to amalgamate the aluminum. The solution is poured off and the foil is washed with four one-liter portions of water.
To the amalgam is added, in sequence, 80g of ammonium chloride in 101ml of water, 302ml of isopropyl alcohol (100%), 244ml of 25% NaOH solution, 89g (0.5 moles) of piperonylacetone, and then 588ml of isopropyl alcohol. The mixture is swirled occasionally for two hours, and kept below 60°C by cooling with an ice bath as necessary.
The mixture is then filtered through Celite (a diatomaceous silicate powder which is placed in a layer over the filter paper before filtering, it is sold by chemical companies as Celite), and the filter cake is washed thoroughly with methanol. Combine the liquid filtrates and distill off the methanol (65°C), isopropyl alcohol (82°C) and the water (100°C).
Dissolve the oil in 200ml of ether, and extract the MDA into two 500 ml portions of 3N HCl. The acid solution is washed with three portions of methylene chloride equal in volume to the acid solution (you will probably have to wash portions of the solution at a time unless you have a huge separatory funnel). The acid solution is basified with excess 25% sodium hydroxide solution (red litmus turns blue) and the liberated oil is extracted into three 500ml portions of methylene chloride.
The methylene chloride solution is dried with magnesium sulfate. The drying agent is filtered out and the methylene chloride distilled out. The residual oil is distilled under reduced pressure and the distilled oil then dissolved in ether
(or toluene or methylene chloride). HCl gas is bubbled through the solution until no more precipitate is formed. The precipitate is filtered off and allowed to dry (~70% yield can be expected).
Nichols et al, J. Med. Chem., 29, 2009-2015 (1986).
Obviously don't need that much HgCl2 but.
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