4-Methyl Methcathinone

Kinetic
(hive bee)
Hi bees,
I've been bored over the last couple of days and had a few fun reagents lying around, so I though I'd try
and make some 1-(-methylphenyl!-"-methylaminopropanone hydrochloride, or -
methylmethcathinone as I suppose it would be commonly called# $ompleted within % hours, starting
from toluene# &ach step is a first attempt only, and I've included suggestions for the procedure if I
attempt it again# 'he first two steps work very nicely, but the yield killer is the final step, giving ()*#
However, this still corresponds to a +* yield of product from toluene, so it's not too bad overall,
Preparation of 4-methylpropiophenone 1
-+g aluminium chloride
+..m/ dichloroethane
0m/ propionyl chloride
)m/ toluene
0..m/ iced water
"..m/ )* 1a2H solution
3agnesium sulfate
)m/ ()..mmol, 0g! toluene was added over +. minutes to a solution of -+g ()).mmol! anhydrous
aluminium chloride and 0m/ ()")mmol, 4g! propionyl chloride in "..ml dichloroethane cooled via
an e5ternal ice bath# 'he solution was allowed to stir for a further 1#) hours at ".o$, and was then
carefully added to )..m/ stirred iced water# 'he lower dichloroethane layer was separated off, and the
a6ueous layer e5tracted with "5).m/ dichloroethane# 'he combined e5tracts were washed with
"51..m/ )* 1a2H, 1..ml water, and then dried over magnesium sulfate# 'he solvent was removed,
and the ketone vacuum distilled at 1"+-1"0o$, to give 1-(-methylphenyl!-propan-1-one as a
colourless oil#
7ield, -.#.g (4)*!
Comments: 8ash with +51..m/ )* 1a2H instead of "51..m/#
9$3 should be a better solvent, simply because it is easier to remove under vacuum#
4-methylpropiophenone to 2-bromo-4-methylpropiophenone 1,2
+%m/ -methylpropiophenone
1m/ %* H:r
1m/ bromine
1")m/ glacial acetic acid
0).m/ water
+..m/ dichloroethane
3agnesium sulfate
'o a solution of +%m/ (").mmol, +-g! -methylpropiphenone in 1")m/ glacial acetic acid was added
1m/ %* H:r followed by, over the course of an hour, 1m/ ("-)mmol, g! elemental bromine# 'he
reaction mi5ture, which changed to a nice pink colour during addition, was stirred for a further 1#)
hours, then slowly poured into )..m/ ice-cold water, with swirling after each careful addition# 'he
cream-coloured precipitated product was taken up in "..m/ dichloroethane, and the a6ueous layer
e5tracted with 1..m/ dichloroethane# 'he combined e5tracts were washed with "5").m/ cold water,
then dried over magnesium sulfate# 'he solvent was removed under vacuum, taking care to keep the
temperature below ).o$, leaving a tur6uoise oil, "-bromo-(;-methylphenyl!-propan-1-one, which
solidified almost immediately on cooling, into sparkling wa5y crystals#
7ield, )-g (1..*!
Comments: 'ry and keep the temperature below +.o$ when removing the solvent < coloured crystals
indicate some decomposition (above were a very light colour, so only mild!# 9$3 would be a better
e5traction solvent since it could be stripped off at a lower temperature, causing less decomposition#
2-bromo-4-methylpropiophenone to 1-(4-methylphenyl)-2-methylaminopropanone
hydrochloride 3
1+#)g methylamine H$l in 1)m/ water
-#4g sodium hydro5ide in ".m/ water
11#g "-bromo-;-methylpropiophenone
0m/ +-* H$l diluted with "m/ water
11)m/ toluene
"")m/ water
=cetone
'o a stirred solution of 11#g ().mmol! "-bromo-;-methylpropiophenone in ")m/ toluene held at
".o$ was added, over ) minutes, 0#"g methylamine in +)m/ water (prepared by adding a solution of
-#4g (14%mmol! sodium hydro5ide in ".m/ cold water to a cooled solution of 1+#)g methylamine H$l
in 1)m/ water!# 'he mi5ture was allowed to stir for a further 10 hours at ".-")o$, then was poured
into 1).m/ ice-cold water# 'he toluene layer was separated off, and the remaining freebase e5tracted
with "5".m/ toluene# 'he combined toluene e5tracts were washed with +5")m/ water, and then
acidified with "51)m/ dilute H$l# 'he combined acidic e5tracts then washed twice with ")m/ toluene
and evaporated under vacuum to dryness, allowing an off-white solid to form# ".m/ acetone was
added and was heated to boiling, forming a homogenous solution, which was then slowly cooled,
allowing crystals to precipitate# 'he crystals were filtered and rinsed with around 1..m/ ice cold
acetone#
7ield, #%g ()*!
Comments: 'ry stirring for " hours at .o$, which will inhibit pyra>ine formation# It may also lower
the yield, but I'll see ne5t time I try# It's doubtful (I3H2! that a yield of over ).* can be e5pected for
this third step, because of the side reactions which can and do occur#
7ield given before recrystallisation, but after concentration and re-filtering and washing of the 1..m/
acetone washes, which provided a further 1g of product# ?ecrystallisation is highly recommended to
remove any remaining pyra>ine, and can be done from acetone@methanol#
1 Ateps 1 and " both based on a synthesis of a Byrovalerone analogue, -3BBH, Byrovalerone with a
he5ane chain instead of pentane# 'hanks to our endearing 1emoC'enetur for providing the -3BBH
synthesis#
2 'he intermediate bromoketone is 6uite a powerful lachrymator, even when solid# 'ake care with
washing your glassware after the synthesis, and please don't use hot water until you've thoroughly
washed everything with cold water first#
3 /oosely based on Bost "%41. (foxy2: "Methcathinone and ephedrine from propiophenone",
Stimulants), although I never managed the -.--* yields claimed when attempting this on
bromobutyrophenone#
2f course this product could also be reduced in good yield to -methylephedrine, and then very easily
made into (-methyl!-methamphetamine# If you were to do that, I'd suggest reducing the bromoketone
before adding the methylamine# 'his way, the methylamino group can be added under much more
vigorous conditions, resulting in a higher yield# 2ne attempt at this gave a yield of around 0.*, but I'm
sure it could be increased#
'he bioassay went rather well too# I was a bit scared about what snorting ).mg might do, but since I've
been almost constantly abusing the (badly synthesised! 1-phenyl-"-methylaminobutan-1-one (i#e#
methcathinone with a butyl chain instead of the usual propyl!, ).mg didn't do too much# I thought I'd
wasted my time until I snorted another 1..mg about +. minutes later, and then it hit me# Intense rushes
all over, lasting for well over +. minutes# Aince I have 6uite a high cathinone tolerance at the minute, I
had another 1..mg about an hour later, then 1..mg an hour or so after that# &ach time I could feel the
rushes of energy coming across me, and after that, a fantastic sense of well-being that I haven't got
from any drug before e5cept my beloved ecstasy#
I'm still feeling the effects now, since I only completed the synthesis 0 hours ago, and began the
bioassay an hour later# It's a fun drug, and although less potent than methcathinone (unless my
tolerance is really high!, it's easy to make, and best of all, legalD Hopefully someone will find this of
use, or at least of interest###
?hodium
(Chief Bee)
.-.)-.+ .1,10
1o "+4)+
Conrat!lations"
I'm impressedD 7ou have not only tested a new drug, you have also synthesi>ed it yourself completely
from scratch and written a te5tbook e5ample of what a synthetic writeup should look likeD
I hope that the trend I have noticed here during the last few weeks will continue, there has been several
people posting typed Eournal articles, notes on practical laboratory procedures F e6uipment as well as
more than one really nice post compilation digest ('hose digests feels like a sort of GHive =bstractsG if
you ask me!#
:arium
(ive !ddict)
.-.)-.+ 11,.
1o ".)
#o$"
Hat off for you Kinetic# :alls and brains, what a nice combination# If only you were a woman#
Kinetic
(ive Bee)
.-.)-.+ 11,)"
1o ".0
%e&t mornin'''
'hanks ?hodiumD I already had it written up, so I thought I'd post it in case someone found it useful#
I've edited it slightly, since I now realise I was rather out of it when I originally wrote the post# If I
work out a better procedure for the third step I'll post it, because there was noticeable pyra>ine in the
a6ueous methyl-methcat H$l solution even after washing twice with toluene# 'he 1..m/ acetone
washes removed it, but I'd rather it wasn't there in the first placeH maybe at .o$ less will form#
I think another very similar cathinone which might be interesting is the indane analogue, as tested by
=ssholium, but without a full writeup# =ntoncho posted =ssholium's comments on the final product,
which sound promising, Bost ")"110 (!ntoncho: ""e: Short duration !mphetamins", #eneral
$iscourse)
=nyway, as to what I can remember from last night,
..mg was 6uite alot to take in one evening, but it wasn't too long lasting so I kept 'topping up'# 'he
rushes after each line were ama>ing, and I remember feeling very much like I do when coming up on
ecstasy, but four timesD 'hat beautiful weak feeling, when you Eust think 'oh, fuck, I feel so fucking
good###' It's more euphoric than I remember my first time on the butane methcathinone analogue to be# I
felt very compelled to do things, but I was completely unable to keep my concentration on literature
searches I was trying to do at the time# I had a very strong urge to socialise, and almost went clubbing,
but thought better of it#
=n interesting effect was that although I consumed my final dose of 4.mg only 1 1@" hours before
going to bed, I was asleep within +. minutes or so, and woke up having had about - hours sleepH totally
unheard of for me on stimulants, and more like the way I sleep after taking ecstasy# 'here were actually
some fu>>y visuals when I was trying to get to sleep, but I can't really remember much about them#
'his morning I feel pretty normal, Eust a bit tired# I'm sure once I have a shower and something to eat
I'll be back to normal# 3aybe this could be a candidate for a Ahort 9uration '=mphetamine'I
&dit, 'hanks :arium, although I'm not sure having balls and brains would be such a nice combiation if
I actually were a woman#
Kinetic
(ive Bee)
.-.)-.+ "1,..
1o "1+.
(top Press"
8ell it turned out my acetone washes provided a further gram of fluffy white product after
concentration, washing the rather yellow crystals (pyra>ine contamination! a few times in acetone and
drying# I've edited my post to give the yield after taking this into account, so the overall yield is now
+* from toluene, before recrystallisation### 'hat's good enough for me at
Kinetic
(ive Bee)
.-.)-.+ "1,++
1o "11
(orry
'o keep replying to my own post, but I Eust had an idea which seems 6uite promising if anyone's
willing to try the unusual sounding '-methyl--methylaminore5', and should give very good to
e5cellent yields in each step,
1,"! Jollow my procedure for the first two steps, both good@very good yields#
+! Awap the bromine for an a>ide, should give a good yield, especially since the bromine is alpha- to a
ketone# 'here's probably something in 'JA& for this alreadyH I'll search in a minute#
! ?educe the ketone and the a>ide simultaneously, possibly with sodium borohydride, to form -
methyl phenylpropanolamine#
)! =dapt the standard procedure from phenylpropanolamine to -methylaminore5H should give an e6ual
yield since the methyl group won't interfere#
=ny comments@suggestionsI ?itter has a similar procedure to my steps + and in
https,@@www#rhodium#ws@chemistry@mda#a>ide#html, so they should also work nicely#
2h, and I really Eust have to say a big Juck 7ou to the KK Lovernment and their stupid drug laws,
since I'm high as a kite and there's nothing they can do###
(### sorry, I really had to get that off my chest!
(ive Bee)
.-.)-.+ "+,).
1o "1)4
MitusCMerdegast
(ive Bee)
.-.0-.+ .1,)-
1o "1%%
conrat!lations"""
'his is for you ,
'hat's a wonderful piece of pioneering research, congratulations man DD
$heers D
(ive Bee)
.-.%-.+ "+,"-
1o "%)1
everyoneD
Hopefully there will be more to come, Eust not at the rate :arium manages to post###
(Moderator)
.-.%-.+ "+,)%
1o "%0)
)t $o!ld be interestin to *erify the '''
It would be interesting to verify the 393=-like properties### =re you sure about itI
:arium
(ive !ddict)
.-.4-.+ 1.,11
1o ")."1
+erifyin
I'll make a batch of it too# I've become very curious about this compound#
Kinetic
(ive Bee)
.-.4-.+ 14,"
1o ")1"
Properties
I've never knowingly tried pure 393=, but have had on more than numerous occasions 'ecstasy' pills,
hence I compared it to ecstasy, and didn't use the more specific term '393='# I'm sure however that of
the various pills I've had over the past " 1@" years, at least some were mainly 393=, so I feel Eustified
in comparing the two#
'he first bioassay was written whilst still feeling the effects of the drug# 'he comparison to ecstasy was
comparing the well being and general niceness I felt at the time to how I also feel on ecstasy, so in that
respect, it was like ecstasy# I don't think it was the same as ecstasy, but for me at least there were
pleasant parallels#
'he loved-upness wasn't 6uite as pronounced, but I felt a strong urge to socialise, and I managed to
send a te5t message to a male friend containg 'love and hugs', something I have a tendancy to do on
ecstasy###
'he complete lack of residual insomnia also made me think there was something other than a pure
stimulant providing the rush, after consuming 0..mg (with the final 1..mg taken at about 1.pm! on
Aunday night, I was able to sleep from midnight until 11am with only a few minutes awake in between#
If I give this to anyone else I'll report back on how they like it, but I suspect that :arium will have tried
it by then# I would definitely suggest to try step + at a lower temperature, say .o$, for a longer period#
I'm going to do e5actly this tomorrow (stirring for " hours!, and although the yield may be lower, I'm
pretty sure the purity of the final salt will be increased# If the yield is lower using this modification, I
recommend stirring for a longer peroid with no increase in temperature, because I now know that
heating causes more harm than to aminopropiophenones than it does to the longer chain aminoketones
with the same 1-substituents, which I originally based the synthesis on#
:arium
(ive !ddict)
.-""-.+ 14,1
1o "%-.1
Can it be tr!e,
Here I sat rolling my thumbs waiting for my -methylpropiophenone to be delivered###:oringDD
I suddenly remembered that I had some -hydro5ypropiophenone# 2h boyD I can try the method with
this substrate instead of Eust sitting here looking stupid# Aaid and done# Happliy singing a little tune I
assembled the glassware, gathered the chemicals###Juck, I have no bromineD 1o 1a:r or K:r either#
8ait a second# I have some KI###Has the KI@25one-system been tried for the insertion of iodine in the
beta-position of a propiophenoneI $an't remember that I've seen that#
8hat the hell, I'll try it#
KI ",)g (1) mmol!
'-Hydro5ypropiophenone, ","0g (1) mmol!
25one, 4,"1g (1) mmol!
3ethylamine, 1,)ml of a .* a6 solution (roughly ". mmol!
3e2H
8ater
'o a "). ml roundbottom flask e6uipped with a magnetic stirrer was added ",)g KI, ","0g -2H-
propiophenone, +.ml 3e2H and ".ml water# =ll of the KI and most of the propiophenone went into
solution within a couple of minutes# 4,"1g 25one was added in portions of 1g# 'he temperature rose
after each addition# 'he temperature was allowed to reach to .N$ before mild cooling was applied#
'he color changed from colorless to purplish and some iiodine fumes was visible# 'hen the color
changed to a more red-brown and the temperature dropped back to room temp raplidly# ). ml cold
water wad added to the mi5ture# 'his caused a reddish-brown solid to precipitate which was isolated by
gravity filtration and washed with some water# 'he filtrate had a orange tone#
'he solid was transferred back to the rinsed "). ml flask with the aid of 1). ml 3e2H# 3ost of the
solids stayed undissolved# 1,) ml .* a6ueous methylamine was added with a syringe during one
minute# =lmost immediately the color changed to orange, then to a bright yellow within one minute,
then slowly to a pale yellow and finally after five minutes the solution was thick from colorless
crystals# 9uring the addition of methylamine the temperature went up from ".-")N$# 'he solids was
removed by filtration and dried to constant weight#
7ield ",4g of possible 1-(-hydro5yphenyl!-"-methylamino-propan-1-one hydroiodide#
$an it be this easyI I have no idea yet if those white crystals really are the cathinone# :ut there are a
few signs indicating this# If the iodination attacked the aromatic ring there would be no reaction with
methylamine, and there was# If those red-brown crystals was Eust a mi5ture of free iodine and unreacted
-hydro5ypropiophenone there would be no reaction between the iodine and methylamine, and no
dramatic color change, again there was#
$an someone shoot me down, please# It Eust can't be this easy# . minutes from start to finished
product##
Jreaky
(ive Bee)
.-""-.+ "1,)0
1o "%-+1
- ca!tio!s .$o$."
8ow, e5cellent :ariumD 8ithout Eumping to conclusions of course it certainly sounds like you've got
something at least resembling the cathinone#
I wouldn't be surprised at all if the methylamine reacted as 6uickly as it did# It reacts rather 6uickly
with the alpha-bromoketone, so the reaction with the iodoketone should be even faster#
I do have one suggestion@6uestion of what your product could contain, something I've Eust thought of,
but I hope I'm wrong, 8hat's the solubility of methylamine hydriodide in methanolI :oth of the
methcathinone derivatives I've made have been soluble in methanol, yet this precipitated out of
solution# Aince you used less than " e6uivalents of methylamine, won't any liberated HI react with the
free methylamine in solution before the methylamine has a chance to react with the iodoketone, thereby
giving a mi5ture of cathinone product and methylamine HII 'wo e6uivalents of amine are usually
used, one as the free acid 'scavenger'#
2f course there must be at least as many moles of cathinone as there are methylamine HI, if there is
any methylamine HI at allH no HI will be given off if unless a reaction occurs between the free
methylamine and the iodoketone, so you should have at least ).* product in there# Hopefully I'm
wrong, and you've managed (once again! an e5cellent yield of lovely pure crystalsD It'd bee wonderful
to see such a high yielding simple procedure instead of the two step method I used# Keep us updated
if@when you have the chance to do some analysis of the product
&dit, Knrelated to :arium's work, I made another batch of this at the weekend, but changed the workup
slightly# In step +, once the off-white solid is obtained, it should be rinsed thoroughly with cold 'HJ,
which it is insoluble in, to remove all the yellow@orange pyra>ine# 'he white crystals can then be
dissolved in methanol@acetone, and once crystallation is complete, a purer product is obtained than by
the previous method of recrystallising twice from acetone without the 'HJ wash#
=nother point to note is the rather rapid build up of tolerance# Jor me at least, the 'ecstasy-like' feelings
I noted the first couple of times I tried it are pretty much gone# Oust to serve as a warning really, -
33$ is 6uite a bit less potent than most other stimulants, and isn't suitable for marathon tweakingH I
found myself taking 1..mg appro5imately every hour after a couple of days solid use# I still stand by
what I said about the first week I tried it though, Eust be aware that it won't lastD 'he first couple of
times were e5tremely pleasant, although a little short lived# 3aybe eating it would be wiser for a longer
lasting high#