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Author Topic:   Who needs methylamine anyway....
Modesty
Member
posted 02-10-99 01:42 PM     Click Here to See the Profile for Modesty     
UN-FUCKING believeable....

Remember that thread from a few days ago -"Ritter Al/Hg nitro variation"? If not, well - it's a few lines down from this one.

After sitting for about 48 hours (did not damage the goods) the dream was able to be continued..

Extracted the goodies from the Al/Hg/NaOH sludge that refused to separate. Dried the litre of toluene, cooled it and when it was crystallized, this non-chemist was blown away by the mass of sparkling white crystals that appeared. Looks like the stuff from the NaBH3CN rxn!

It's not dry yet, but it must be close to 40g, will get back on that one.

The thing is I thought I had fucked up! Using thin foil, everything was spent after 1.5 hrs. of refluxing Some heat was applied after about an hour, and it was left stirring for a total of 3-3.5 hrs. Nitromethane was 100% from drag racing fuel. Damn nice fella sold it to me for next to nothing. There was no "reddish color" to the extract btw.

Ritter - let me kiss your feet...

Love, Modesty

boingo
Member
posted 02-10-99 02:43 PM     Click Here to See the Profile for boingo     
What sort of stirring was hypothetically
used for this reaction?

peace,
boingo

Modesty
Member
posted 02-10-99 02:54 PM     Click Here to See the Profile for Modesty     
No stirring. Never had much success with stirring these Al/Hg procedures anyway. Never got such clean product from them either. Smooth. Bioassay is being performed as I am writing. Hubba Hubba :-)

Mod.

boingo
Member
posted 02-10-99 03:35 PM     Click Here to See the Profile for boingo     
awesome. now get off the computer and go have some fun!!!!
congrats. the vindication of ritter is at hand!

peace,
boingo

Getafix
Member
posted 02-12-99 08:00 AM     Click Here to See the Profile for Getafix     
Hey Modesty

Mind giving us a complete write-up? would be appreciated


-getafix

Bacchus3_4
Member
posted 02-14-99 04:16 PM     Click Here to See the Profile for Bacchus3_4     
I second the motion in favor of a complete and easy to follow (hypothetically of course, and solely for academic purposes) write up.

40g nicely done!!!

------------------
Bacchus

Modesty
Member
posted 02-16-99 09:04 AM     Click Here to See the Profile for Modesty     
I would not mind giving a complete write-up except that I have very little to add to the procedure as it was done exactly as described in TSII. And due to the fact that selling this book is the source of income of our host here.... But be my guest, buy the book :-)
The final yield of dry hypothetical hcl was 34g. With real thin foil, the rxn was refluxing hard with a condenser on top. Yield will be better next time with just a little thicker foil. (Not too thick though, because the stirring will be needed again, just enough to keep the reaction going for another hour or so.)

This has been some weekend...


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