So for the MDA rxn using 28% NH4OH in a Pipe Bomb, I am specifically referring to this ref from "The Secrets of Methamphetamine Manufacture,":

To do the reaction, 50 grams of the bromo compound is poured
into a beaker, and 200 ml of concentrated ammonium hydroxide (28%
NH3) or 40% methylamine is added. Next, isopropyl alcohol is added
with stirring until a nice smooth solution is formed. It is not good to
add too much alcohol because a more dilute solution reacts slower.
Now the mixture is poured into a pipe "bomb." This pipe should be
made of stainless steel, and have fine threads on both ends. Stainless
steel is preferred because the HBr given off in the reaction will rust
regular steel. Both ends of the pipe are securely tightened down. The
bottom may even be welded into place. Then the pipe is placed into
cooking oil heated to around 130 C. This temperature is maintained
for about 3 hours or so, then it is allowed to cool. Once the pipe is
merely warm, it is cooled down some more in ice, and the cap
unscrewed.

     The reaction mixture is poured into a distilling flask, the glass-
ware rigged for simple distillation, and the isopropyl alcohol and
excess ammonia or methylamine is distilled off. When this is done,
the residue inside the flask is made acid with hydrochloric acid. If
indicating pH paper is available, a pH of about 3 should be aimed for.
This converts the MDA to the hydrochloride which is water soluble.
Good strong shaking of the mixture ensures that this conversion is
complete. The first stage of the purification is to recover unreacted
bromo compound. To do this, 200 to 300 ml of ether is added. After
some shaking, the ether layer is separated. It contains close to 20
grams of bromo compound which may be used again in later batches.

     Now the acid solution containing the MDA is made strongly basic
with lye solution. The mixture is shaken for a few minutes to ensure
that the MDA is converted to the free base. Upon sitting for a few
minutes, the MDA floats on top of the water as a dark colored oily
layer. This layer is separated and placed into a distilling flask. Next,
the water layer is extracted with some toluene to get out the remaining
MDA free base. The toluene is combined with the free base layer, and
the toluene is distilled off. Then a vacuum is applied, and the mixture
is fractionally distilled. A good aspirator with cold water will bring
the MDA off at a temperature of 150 to 160 C. The free base should
be clear to pale yellow, and give a yield of about 20 ml. This free base
is made into the crystalline hydrochloride by dissolving it in ether and
bubbling dry HCl gas through it.

I forsee problems with that much water in the rxn, but I wanted to know if anyone here had ever experimented with this technique (Jon). I was re-reading the bromosafrole write-up by Uncle Fester in the back of 'Practical LSD Manufacture,' a book which I know has so much bullshit in it, but he talks about preparing a 20% alcoholic solution of Ammonium using the gas or CH5N by gassing before using the Pipe bomb. He also specifically mentions problems with water with this technique for the amination....

Any input is greatly appreciated here.

_Pbinteger.

ImAMANGUYS:

Would you post pics of the free base extract ?

_Pbinteger_

Absolutely sir. I'll be working it up tomorrow or the following day and will post pics immediately following for your viewing pleasure

As it pertains to the amination you seem to be overcomplicating the matter and also refering to an outdated process (not sure about that). This may be why Jon or other more prominent members have yet to respond to your question  I assure you this reaction Jon suggests isnt a hard one provided you keep it dry and have the required materials. PM me if you need more help and I'd be happy to give it. Perhaps send me a picture of your gassing generator and setup?

Wishing you the best and will post soon 

Hi

I am definitely going to run jon's route again.. I'm waiting on more 99% IPA to arrive.

I was just curious if anyone knew if that write up would even actually work. Seemed kind of iffy to me with NH4OH...
I know Uncle Fester is notorious for write-ups that just don't work...
I was just curious if anyone had tried it.

Jon,

I just finished another bromosafrole rxn. I noticed two distinct layers upon the initial crash with H2o. the first was deep red and crashed straight to the bottom. Above that was a bit of water and then a yellow layer (which I wrongly assumed was entirely unreacted safrole). I worked up each layer separately. The deep dark red layer is certainly bromosafrole -- the work up was as expected. The second layer formed tough emulsions and smelled just like safrole. I was able to isolate it, clean it up and store it in DCM over Na2so4. After a day in the fridge, and some more emulsion breaking, It took on the familiar bichromatic green hue that you would expect from rather dilute bromosafrole. So I am again assuming that there is unreacted safrole acting as a solvent to the slightly heavier halosafrole. Would it be worth it to separate the 2 with fractional distillation? If there were fewer moles of halosafrole in a solution of safrole, and you ran the anhydrous methylamination with the entire volume, it seems it would only help the reaction go more quickly if the stoichiometry was prepared assuming the entire volume was bromosafrole.

Thoughts?

Is this the correct math for 15% w/w of IPA?

((Xg CH5N / 15%) (85))/0.786g/cm³

ImAMANGUYS,

any news?

how much base was obtained from  how much iodosafrole? I mean what were your yields?

So I've been thinking about this threads original question, "why not straight to iodosafrole?" and I realized why the attempts to substitute KI/NaI in the reaction don't work well. You simply need to switch your acid to phosphoric acid, the sulfuric acid oxidizes it to elemental iodine which is likely interacting mostly(thankfully) with the GAA, leaving lots of unreacted safrole. Also I was slightly perplexed by the use of the GAA as a solvent until I realized it's to clean up the alkali metals from the reaction, but I'm not sure if this reaction can work with H3PO4 due to the low temperature and water contained in the acid solution.

You are right it will not work this way. For in situ HI production you would have to use 90-95% H3PO4, temp. 115°C up. But what speaks actually against this? H3PO4 is easily concentrated by boiling away the water and strong stirring circumvents any solubility issues (say: it doesnt matter at all how much the compound will dissolve).
But you want the iodinated compound?
Then you are all barking at the wrong tree...

From the ephedrine reduction you should know that HI will reduce your iodinated compound to the hydrocarbon, how do you intend to stop this? I tell ya, you cannot, and thats why this is just bullshit.
Plain iodination would call for Phosphorus tri-iodide and strictly anhydrous conditions (HI iodination generating water, logically).

regards
/ORG

The honored WizardX and I have had different opinions on quite many things of chemistry a long time.
I am not going to say I am always right.
Different people in different set and settings make obviously different rules of reactions.
What I say is though that in my part of the world, my set and setting I am usually right.

Maybe you check your location before trying something 

good luck
/ORG