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Methamphetamine via Reductive Amination of Phenyl-2-


Propanone
Using Aluminum Amalgam and Methylamine in wet Isopropanol
Procedure adapted from the synthesis of MDMA from MDP2P in Pihkal #109
Procedure 1: Using Methylamine ydrochloride
In a 1000ml wide-mouthed rlenmeyer flask! 19 "rams of aluminum foil cut to #$#cm pieces
was amal"amated in a solution of %00m" mercuric chloride &'"(l2) in *00ml warm water until
the solution +ecame "reyish! and hydro"en +u++les was e,ol,ed in a steady rate from the
aluminum surface- .he water was decanted off! and the aluminum amal"am was washed with
2$%00ml cold water-
.o the aluminum amal"am there was added 29-%" methylamine hydrochloride &0-// mol! # e0,)
dissol,ed in #0ml hot water! *% ml isopropanol! *0ml 2%1 a0ueous 2a3' &0-// mol)! 19-*%"
&0-1/* mol) phenyl-2-propanone &P2P) and finally 1*%ml isopropanol- 'ydro"en was ,i"orously
e,ol,ed from the aluminum amal"am! and the temperature of the solution rose 0uickly- .he
reaction rate was controlled +y immersin" the reaction flask in cold water durin" 2h! whereafter
it was allowed to stand at room temperature with ma"netic stirrin" o,erni"ht! with attention
+ein" "i,en to the reaction mi$ture durin" the first hour so that the temperature did not rise o,er
%04(-
.o the reaction mi$ture there was added another %0ml 2%1 2a3'! and the reaction mi$ture was
stirred for #0min and then allowed to settle- .he clear supernatant was decanted! and 100ml
isopropanol was added to the "rey slud"e! and it was stirred for 1%min! and the supernatant a"ain
decanted- .he aluminum slud"e at the +ottom of the flask was now filtered throu"h celite in a
+uchner funnel and washed with 2$%0ml .'5 &methanol can also +e used)- All the decantations
and washes were com+ined! and the solution concentrated under ,acuum-
.he residue was taken up in 1000ml water! acidified +y the addition of conc '(l! and washed
with #$%0ml D(M! +asified with 2%1 2a3'! and e$tracted with #$100ml D(M- .he com+ined
D(M e$tracts were dried o,er M"63/! filtered and the sol,ent distilled off- .he residue was
distilled twice under aspirator ,acuum at 100-1104( to "i,e 1/-7%" &7*1) of methamphetamine
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free+ase as a water-white oil- .he hydrochloride salt can +e prepared +y dissol,in" the oil in 10$
the ,olume of diethyl ether and "assin" the solution with dry '(l "as until no more precipitate
forms- .he methamphetamine hydrochloride is filtered off with suction and washed with diethyl
ether and air dried-
Procedure 2: Using !"# A$ueous Methylamine %ree&ase
In a %00ml wide-mouthed rlenmeyer flask! aluminum foil &10"! 0-#* mol) cut to #$#cm pieces
was amal"amated in a solution of 200 m" '"(l
2
in /00 ml warm water until the solution +ecame
"reyish! and hydro"en +u++les was e,ol,ed in a steady rate from the aluminum surface- .he
water was decanted! and the amal"amated aluminum pieces were washed twice with 2%0ml cold
water-
.o the aluminum amal"am &still in the a+o,e flask) there was added! 0uickly! a /01
Methylamine solution &/# m8! 0-%0 mol)! isopropanol &100 m8)! Phenyl-2-Propanone &1#-/2"!
0-10 mol)! and finally another 100 m8 isopropanol &which was used to rinse the +eaker the P2P
had +een in)- .he aluminum pieces were poked with a "lass rod so that all of them were +elow
the surface of the li0uid- 'ydro"en +e"an to e,ol,e ,i"orously from the aluminum surface! and
the temperature &which was measured +y a small thermometer inserted into the flask) rose
0uickly- .he e,aporation of methylamine was attenuated +y co,erin" the mouth of the flask with
some Al foil &do not plu" it ti"ht! or it may e$plode)! and the reaction rate was controlled +y
immersin" the reaction flask in cold water from time to time durin" the first hour so that the
temperature did not rise o,er %04(- At the 2 hour point most of the aluminum was consumed!
and 20 m8 2%1 a0ueous 2a3' was added to the solution and ma"netic stirrin" was initiated
&keep an eye on the temperature a"ain! and keep it +elow %04()- At the # hour point another 20
m8 2%1 2a3' was added &no si"nificant temp rise)! whereafter it was allowed to stir at room
temp o,erni"ht and then allowed to settle-
.he clear supernatant was decanted! 100ml isopropanol was added to the "rey slud"e! it was
stirred for another hour! and the supernatant a"ain decanted after the particle suspension had
settled- .he aluminum slud"e at the +ottom of the flask was now ,acuum filtered throu"h an inch
of (elite in a +uchner funnel and washed with 2 $ %0 m8 methanol- All the decantations and
washes were com+ined! and the solution concentrated under ,acuum-
.he residue was taken up in #00 m8 water! acidified with conc- '(l! washed with #$%0ml
methylene chloride! +asified with 2%1 2a3'! and e$tracted with #$100ml ethyl acetate- .he
com+ined or"anic e$tracts were washed with *%ml +rine! followed +y dryin" o,er anhydrous
sodium sulfate with "ood ma"netic stirrin" for 1% min- .he dryin" a"ent was remo,ed +y
filtration from the crystal-clear solution and the sol,ent distilled off on an oil-+ath heated to no
more than 1104( &as to not risk any e,aporation of the free+ase)- .he residue was taken up in
1%0 m8 diethyl ether and with "ood stirrin" a solution of %M '(l in isopropanol was added until
the solution was acid to dampened uni,ersal p' paper- .he precipitate was filtered off with
suction usin" a fritted "lass funnel and the filter cake was washed with 2 $ %0 m8 ether and
sucked dry- After air-dryin" o,erni"ht on a plate! the crude product &1#-7 ") still had a stron"
sol,ent smell! and was recrystalli9ed +y dissol,in" it in 7% m8 acetonitrile &% m8:"ram)! and
0uickly ,acuum filterin" the hot solution throu"h a fritted "lass funnel to remo,e a sli"ht
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tur+idity! and the solution was then left at room temp to crystalli9e! and after a+out an hour the
white crystalline precipitate was filtered with suction! washed with 2 $ 2% m8 ether and air dried-
.he filtrate and ether washes &collected separately) were +oth cooled to -204( in the free9er! and
from the acetonitrile a second crop was collected! while nothin" came out of the ether-
.he first and second crop wei"hed 12-0 " and 0-/% "! respecti,ely! makin" the total yield of
Methamphetamine 'ydrochloride 12-/% "rams! or 7*1 of theory