al/hg nitromethane question

[ekolo]

just a quick question is it ok to use Pie pans aluminium
in an Al/Hg nitromethane reduction. i mean is the aluminum Reliable as reynolds alu. its imposible for me to get some reynolds. thanks.

[silenziox]

How about if you give it a try on a small batch and give us
a report if it worked or not?

I'm experiencing similiar problem on red.amination.. I have
some 2,5-dimethoxyphenylacetone (2,5-diMeO-p2p) and I'd like to reduce it to 2,5-DMA having good yield without the need to go via oxime route.

NaBH4 reduction is out of question (unless it forms stable imine?) but I could do Zinc amalgam reduction (any ref's?), or Zn-Ni reduction..

I've spent my last LAH and won't buy anymore of that stuff,
and I don't want to do Pd/C reductions.

So maybee I'll try Zinc/Ammonium formate reduction and Zn-Ni reduction.. Or Zinc-Ni-Tin/Ammonium formate.. Report afterwards.

[ekolo]

yes i am going to do it anyway but just wanted to se if someone has tried it out with pie pans alu before. will be reporting afterwards thanks for the help.

[ApprenticeCook]

swim has had a dream in the past with some alu pie tins for the Al/Hg it works the same way, swim has found though that a bee would just have to use a little more alu pie tin than its reynolds wrap counterpart, swim just puts in ~10% more pie tin than reynolds wrap amount required, seems to work fine.

[cublium]

pie tins work perfect,they are bit thicker so rx runs slower but that's what we are after,no?

[BieneMaya]

Anyone knows this barbeque alu for one time roasting?

It´s a thick alu foil with ~70 mics.
Should pretty work the same...

[abolt]

I have a question.

Bees are told that the use of thicker Al is the way to go for safer, less exothermic reactions, that will not gobble up the Al too quick and therefore lead to a complete conversion of the ketone.

This makes good sense.

Bees are told to add the nitromethane first, in order to have an excess of methylamine available to react with the ketone.

This makes good sense.

My question is.......is the formation of methylamine from nitromethane slower also, now that thicker aluminium is used?

If one were using say 300 micron Al "flashing" would it be wise to wait for a period of time (say 1 hour) after the addition of the nitromethane, to add the ketone?

[ApprenticeCook]

Bees are told that the use of thicker Al is the way to go for safer, less exothermic reactions, that will not gobble up the Al too quick and therefore lead to a complete conversion of the ketone.

Yeh, swims runs a fair amount hotter, but its still managable, just not as subdued as methylman's and gonzo's pages say... as swim said if one uses ~10% more alu foil when using the thinner bbq plate things instead of raynolds wrap it makes it a bit better, swim used to have a fair amount of ketone left over until he realised this....

is the formation of methylamine from nitromethane slower also, now that thicker aluminium is used?

Maybe.... swim thinks there is a balance, to thin and the reaction is out of fuel before you get all the ketone in, and left with heaps unreacted as swim used to... to thick and it runs to bloody slow.... raynolds wrap is a good middle ground, but swim thinks if you had thick stuff and cut it and balled it into really small pieces it should even it out??

[ekolo]

i just made that test with pie alu.

i did 2 test in 2 smal pyrex glases i pored in 100ml of methanol pure grade HPLC in each of the two glases.
then came the HgCl2 in each small amount ofcourse gave it 5min to dissolve.
then because there was no water in my methanol i added some 10ml of dem. water.
now i had only two tests one for pie alu another one is the reguler alu i could find house hold one.
tok few grams of each and throuw the one alu in one glas and other in well other glas . 2min after the pie alu began reacting small bubles everywear the reguler alu nothing.
after exactly 5min the pie alu was heating up the reguler stil nothing odd. i tok 5ml of pure nitromethane and poured in the glas with reguler alu nothing happened hmm maybee something went wrong. but when adding the nitromethane to the glas with pie alu the reaction got hottere(reflux hot) the pieces floated and dissolwed rapidly the solution got steelgrey like and on the bottom was grey sludge.
i think i am going on with the pie alu hehe .

 pie alu thickness: unknown had no time to test it sorry.

[abolt]

[ApprenticeCook]

Pie tin alu, dont know the thickness but if a bee goes to the supermarket and looks for the tins which are throw aways for bbq'ing.

Pick them up and bend them a bit, they should be fairly stiff... swim finds the throw away alu baking trays (big alu tray size to fit a roast) with the other wraps and normal alu foil in the same isle...

Only problem is cutting them up for the grinder... cant count the amount of times swim has cut fingers (esp the webbing between your thumb and pointer! owwww) on this stuff getting it ready but its easy once you get the technique down...

Works fine for swims dreams...

[wyndowlicker]

Hey now,


 Ive almost exclusively used rens aluminum foil now I use diamond.I really dont see the difference in thicker or regular thickness on yields.I think its the procedure for addition thats key.Just for the hell of it Ill post my way.
Always use only 25 grams of foil instead of the 26.5 MM recomends.Ive found you get no residual aluminum flakes that way.Add to your already mixed (1hr)hg/meoh mix.Let mix till dirty gray MeOH starts to appear.Then add 4-5 ml of Nitro.drip in.Wait till it reaches a nice hot temp.Then add the rest of the mix.Wallah!I get grate yields 24 grams before recrys.This works fine on the scale up.Always did get a better yield form H*** than anhydrous MeOH.Even after adding 10ml of DH20.
  Also VL and I one time were trying a bucket reaction of??? I forget the scale up now.So we got some al wire and started to cut it up into little rings.Finally we began the reaction and it was just so slow and got so thick.The reaction actually succeded after adding excessive amounts of MeOH.Had a good 10 grams of wire left over.Actually,After tartrating it in the bucket it made these monster chunks.I was so proud we didnt launch that reaction on my ceiling.We had to stack 4 condensers almost to the roof.WHooo!WHoooooooo!Those we the days.