dormouse (Member)
04-22-00 22:09
No 108662
      Pseudonitosites = OTC #0 -The Cook  Bookmark   


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Author  Topic:   Pseudonitosites = OTC #0 
The Cook
Member   posted 03-01-99 08:30 PM          
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Posting that subject may be a little bold, but I've heard some wonderful fairy tales concerning Bruckner's method. It's time to open a serious thread on this subject, and it's applicability.
I remember a scary tale of N2O3, that left many bees uninterested or irritated. This method is less than amazing ONLY because of the need to generate N2O3, an enormously dangerous gas.
If you've had any experience with those hellish red fumes, you know that ordinary ventilation is NOT adequate. This would be an OUTSIDE dream, on a windy day, in the middle of nowhere. So under those conditions, bubble away. Any other time, use the biphasic phun of Bruckner's method.
The story of this reaction proceeded as expected (Details if you want-else i'll save space on the tempermental hive). Here are some things you might want to know though. (About the story I read)
-The GAA method(Toennies) is another producer of large amounts of N2O3. It was actually interesting, as it took a moment for the initial cloud of fizz to go red, giving me quite a start as I slammed the fume hood window down, and raced for the fan switch. The fairy tale didn't recommend it.
-The next chapter was about a theory to create the alkyl hydrogen sulfate ala the MDP2Pol doc, then swap with NaNO2. This also created a bit of smog, and tended to get too hot. Once it was performed in 100ml of cold ether, but the Nitrite needs to be soluble, I believe. About 18%, but the major byproduct is iso-not-safrole, which can be reused for Bruckner's method. Silver Nitrite might still work, which would afford a safrole->nitroisosafrole one pot.
-The last chapter was a romance novel about an H2SO4 drip, into NaNO2 in water, and safrole in ether. A beautiful marriage took place, affording 4.4g b-nitro as orange crystals from 10g oil (<>%70 safrole). Again isosaf is the side product. Which may be cured by further addition of H2SO4??? I only state that because the story told of a foolish experiment where after the inital addition and several hours of cooling, a good deal of red remained in the ether layer. A short (10ml) H2SO4 drip was performed, and on each drop of the acid, the characteristic monomer cloud was noted. (looks like cupric carbonate slush-dark green, maybe even slightly blue). That drip pretty much cleared the ether layer, and things looked good.
I never got to read the rest of the story, maybe soon, maybe never. How interesting does this sound? We need a trick new method.
-cook
 
Piglet
Member   posted 03-02-99 03:20 AM          
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Sounds good: Complete lab-prep?
 
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