02-06-02 15:41
No 265954
.3mm al foil, into shards with a guillotine, 1L of methanol/100g MDP2P, 1g Hg(whatever)/L solvent, 1g nitro/1g Al, 1.2g ketone/1g Al. Amalgamate foil, slowly drip in all of nitro over three hours, thenm drip in MDP2P with heating to maintain reflux, after total 12hrs workup as per reynolds nitro method.
less solvent, less flask size, greater yeilds
you work out the details
but it works
trust me i am a doctor
wacka wacka wacka
(Hive Bee)
02-06-02 16:14
No 265963
Have you actually done this. MDP2P and ketone are the same fucking thing. SWIM say this would end up wasting a hell of a lot of ketone. Baal has preety much improved this as much as you can for newbees.
(Stranger)
02-06-02 17:43
No 265999
he seems to be a tad confused.... poor little chap
I love the smell of Ketone in the morning.
(Daddy)
02-06-02 20:07
No 266038
Well, I'll try to write it down a bit more obvious/clear and see where we end then:
You take 0.3 mm thick aluminium foil, cut it into pieces of x? cm by x? cm with a papercutter.
The ratios of the involved chemicals are as follows:
1L of methanol per every 100g MDP2P (ketone),
1g Hg(whatever salt) per Liter solvent (MeOH in this case),
1g nitromethane per 1g Al,
1.2g ketone per 1g Aluminium foil.
Amalgamate the aluminium foil with the Hg salt,
slowly drip in all of the ketone over three hours (drip in the MDP2P with heating to maintain reflux) [PERHAPS HE MEANT TO WRITE IT THIS WAY??] , after total 12hrs workup as per reynolds nitro method (what the fuck he means with that? MM, Baal, Osmium, WHUT?).
less solvent, less flask size, greater yeilds.
So, let's see where that leads to for example with 120 gram ketone (MDP2P):
120 gram ketone
100 gram Alu foil
100 gram Nitromethane
1200 ml Methanol
1.2 gram Hg salt
Doesn't sound so crazy anymore if seen by the light of reasonable doubt, ain't it?
What I do not like however, if methods are proposed for the sheer purpose of convincing other members to try something out which is not performed by the writer, but what he would like to see if it works, so the risks and costs are carried by someone else, and the proposer just hopes he gets an enthousiastic answer when one of the next posters confirms that the method really works.
This is the most hidious way of proposing a method: as if it's already done with good results.
I don't know if this goes for the thread writer above, but he can at least give some more details to convince the occassional reader of this thread of his good intentions.
And try in the future to write a bit more clearer and coherent. LT/
WISDOMwillWIN
(Hive Addict)
02-06-02 20:11
No 266041
But he's a doctor! Don't all doctors know how to make drugs?
there must be an answer for everything, if only you knew how to set forth the questions
(Newbee)
02-06-02 23:38
No 266135
The trick is in the detail, how do you get it to stir, yes i use this method, yes the yeilds are great (molar yeild around 80-85% depending upon your patience)
for all you morons who don't realise this is the same reactant fucking ratios as with the reynolds methods but with less solvent, so you don't need a 200L QVF flask to make a decent amount in one go. I use a 20L PE bucket for this, doing 500g ketone runs, and a dry ice condensor (a dry ice condensor is a piece of stainless pipe with mesh on one end, pellets of dry ice are placed on the mesh, no water, no ice, no pumps, no hassels and enormous condensing capacity.
I have had the solvent ratio up to 1.7L/100g ketone also.
As for those who choose to criticise, you make me laugh, you are the ones not doing any fucking experimenting because you are too stupid to even figure out the detail in my little post, so fuck you.
Laptop that obviously doesn't apply to you because you figure out the detail, you are very generous
wacka wacka wacka
(Junior Service Representative)
02-06-02 23:56
No 266144
We all bow down to you, Dr. wacko...
<that says it all>
PB
BTW,
(Daddy)
02-07-02 23:09
No 266626
So why did you choose for a higher solvent/ketone ratio, 1700 ml/ 100 ml ?
Was it because the refluxing methanol was freezing on the dry ice chunks used in your home made reflux condenser ? (Btw, another very interesting idea, if I may say so in this circle of wisdom wizards)
And you had to wait for all the CO2 to disappear before the frozen MeOH dripped back in the solution?
Did you ever see methylamine gas freeze on the dry ice? Very important, if not, then this would be the favourite way of refluxing solutions with methylamine gas in it. Hmmmm, Interesting indeed! LT/
WISDOMwillWIN
(Newbee)
02-08-02 05:26
No 266740
The dry ice reflux condenser really shines in the performic step.
Because of the low temperature differential between the use of ice-cold water in a reflux condenser and the bp of DCM, holding this reaction down was usually a case of very slow performic addition, however with the dry ice reflux condenser instead of an icewater cooled one, your capacity to condense is enormous and the dcm goes back in nice and cold.
The acetone idea is good, but solvent pumps are sometimes not the cheapest things to come across.
The solvent ratios are sometimes higher because the stirring technique I use means i need greater volume to properly cover the aluminium.
editted a little bit for better understanding of the former text, LT/
wacka wacka wacka
(Stranger)
02-08-02 11:25
No 266869
Where would one go about finding a pump that could handle acetone? Are there any (ex.aquarium) water pumps that could dupe satisfactorily or is there a reason that wouldn't work?
Flip
(Daddy)
02-09-02 07:09
No 267309
A simple alu piston pump, something like a miniature plane motor.
Cleverer is to use a dry ice trap, made for that, fill it with acetone/dry ice mix. LT/
WISDOMwillWIN