OK. Today I began a venture to try and use OS Al sheeting method with nitro. Unfortunately for me, the only thing I lacked was the overhead. Which didn't prove to be that much of a nusance, but called for more meoh in the reaction.
I will give the fine details when I am finished but before that I will give some broad details. Suggested by a well known bee here... basically this is how it has gone so far. The ingredients:
86g ketone
61g Nitro
75g al sheeting
1+ml Meoh
First, added the al to a 3L FBF and covered with approx 1L meoh. Added 1.2g HgCl2 and let go for 30 min. Solution turned med grey. After the 30min period, I added 30.5g of the nitro to an addition funnel and set up for reflux on the 3L, and with the addition funnel. I droped, one drop per second or second and a half, the nitro into the meoh/al/hgcl2. This took less than an hour, but I let the reaction run 2 hours...during which time the mixture got exothermic and refluxed fairly hard. After two hours, the reaction cool quite a bit, but still at a slight reflux. Then, into the addition funnel I added the remaining nitro (30.5g) 86g of mdp2p, and approx 20ml meoh. Started this at a very slight drip. The drip was finished in approx 2-2.5 hours. While the reaction only refluxed slightly, as I had to add heat as well. This was all done with a mag stirrer which gave many problems to keeping the mixture stirring. There was much shaking and swirling to try and catch the stirr bar....eventually I found myself adding approx 1.5L to 2L meoh, just to keep the thing stirring for more than a few minutes...At this point the reaction will continue, I'm sure, for an unsepcified time...which at the end, I will give the details. I am under the impression that the reason for the intitial nitro drip is to make availible for the next step, our precious MeAm...which, btw, during my swirling trials, the condenser came loose, and there was an immense smell of MeAm, for sure. The reaction, looks good and sure seems to be doing its thing. 4 hours into the reaction and there are still large al pieces however, it seems as though the majority of it has turned into your typical al sludge, slightly bluish grey.
SO, anyway...I wanted to discuss some further liknesses with this reaction and the typical MM reaction. First, I would like to clarify that the only reason a 12L FBF is used for 200g reactions, is because granny likes to save all that head room, so that basifying can be done in the same flask, therefore leaving begind her the work of trying to get the sludge out of one flask and into another. or into a sep.
Secondly, I would like to take a look at the ratios here for each reaction.
with 150g of al sheeting you can use more or less 180g of tone.
with 150g of al foil you can use more or less (according to MM write-ups) approx 130g of tone...although, I am sure as you upscale, you can use less al as in the sheeting method...only with this bees experience, he has always just added equally to the ratio's when upscaling...never thinking that it is a good possiblilty that when you upscale this rection, that it will probably not need as much al as does the smaller 1x al/hg per MM.
The only real difference between these two, and upgrading each, is the overhead stirrer. I learned that today when trying to stir the sheeting with my magnetic, and realizing that it wouldn't.. I had to add another 1.5-2L of meoh. So, for this 86g reaction, I still needed approx 3L meoh....and in a past 130g reaction FOIL style, I had to use 4L to keep the thing stirring....so the difference is still quite the same....if I had an overhead and wanted to do the foil method, I could definately use less meoh...and I probably wouldn't have to use as much al when I upscale...I imagine, with 150g of al, I could get very close to using 150g of tone using the foil method...therefore allowing me to have a much bigger reaction in a smaller flask...
In my 200g reaction I use 225g of foil, 6.5L meoh...although, the foil could for sure be cut down, just never tried it, and if an overhead was in place, you for sure wouldn't need as much meoh, therefore allowing you very close to the same amounts and volumes as the sheeting method.
Now, I am not trying to pick a fight and shit, I have just now see both done, and both a very much alike, no matter which way you look at it. At this point, I would not be able to agree which is better without getting an overhead stirrer to test my own theories out.
Shit, I got to get me one of those overheads.
DEM
Got another one coming!
If some of us were not so far ahead, the rest of you would not be so far behind!
