Results from Eph HCL + HI ---> OPINIONS WANTED!

[biotechdude]

After success with hypo and I2 rxns, Swix tried a new OTC method to reduce Eph HCL in the presence of excess 57% HI acid using no P-based recycler.  Eph was to be obtained from ephedra plant, and the HI was to be created using phosphoric acid and KI.  No P based recycler was wanted as these are very hard to come by in my area.  However, i was dissapointed with the end result as from 12grm rxn only 3.5grms of 'non-meth' was obtained.  Please note Swix's lab skills are competant, so mechanical error of that magnitude is unlikely.

Basic rundown as follows

1) Steam distilled ephedra to obtain clean white Ephedrine HCl (along with other alkaloid HCL's obv).  [all good]

2) Created HI acid via Argox (from Rhodium.ws) and 'Reference on HI reductions' thread; using Phosphoric acid and KI.  It created a dark red liquid, that heavily fumed when exposed to air.  Density 1.8 - indicates greater than 57% HI con.  [all good]

3) Placed 12 grams Eph HCL in 500ml rbf with condensor atop an oil bath/mag stirrer combo.  75mls of 57%+ HI was added and stirred heated slowly until a nice steady reflux was established at ~125`c inside flask.  This was refluxed for 10 hours and then left to cool for 4hrs.  It was coloured black for the duration.  [maybe good, does large excess of HI and free I hinder rxn?]

4) After cooling, 2.5x the volume of dH2O was added and then lightly boiled for 5 mins to remove any volatile nasties.  Then 2 naptha washes were done (came off purple coloured) which lightened the black colour to a dark red.  During this process, the black sludgy-like iodine precipitate was removed as it clung to the sep funnels walls during filling/pouring.  [unsure if iodine precipitate contained some goods]

5) 200mls of heavily based NaOH solution was added to liberate fb meth. pH was ~13, and solution smelt good (fishy) but different to what was used to.  Upon adding the NaOH solution the rxn fluid turned to a light yellow and had little yellow floaties on top (maybe NaI) and what appeared to be an oil layer (hard to see).  This was steam distilled using external steam source and 400mls distillate was obtained.  The distillate had an oily droplet layer at the start but then disapeared once more water diluted it (almost like Eph steam distallate). 

6) All the distillate was cooled and carefully pH'd to 7 and the whole contents put in a open-doored oven at ~75`c.  This evap'd to reveal dry fluffy bright white (non-clear) salt/crystals.  It tasted different to Eph HCL (more fishy than planty), and only 3.5grams was there (12g was rxn'd).

7) This was recrystalised using hot methanol, acetone added, cooled in freezer overnight and revealed much the same as in 6).  At this point i was not happy and puzzled.

Can any knowledgable Bees shed some light on what may have went wrong.  Theoretically this should work as a very large excess of 57% HI was added at the start (75mls) and only had to reduce 12grms Eph HCL.  Please note Swix does not want to use a HI-recycling agent.  Swix guesses what was obtained was half reacted Eph, however shouldn't more than 3.5 grms have come out as unreacted? Perhaps as Eph doesnt have as strong affinity for steam as meth, more distallate would've need to be collected.  However, if it was meth; 400mls would of been plenty for 12g rxn.  Bioassay indicated it wasnt meth, but still felt nice and floaty.

My thoughts for success include-
* Modified rxn time, reflux temp [strongest hunch] 
* More/less HI, perhaps it was too concentrated (causing overshadowing side reactions)
* The adding of Copper filings to precipitate free iodine as CuI to clear up the solution. Or someother clearing agent
* Swix has lost his touch and he should become a travelling gypsy dancer...

Sorry to be sooo long-winded, thankyou for your time and replies.

[biotechdude]

Upon further UTFSEing, Swix came across the '57% HI sans RP rx help / question ' thread. 

The Wizard explains that the P-less HI/E rxn works in theory if the correct molar excess is used.  However, in reality; factors from HI decomposition, side reactions and competition make this a messy mix in the end. 

So, should Swix pursue pre-made HI/mbRP methods or has anyone on the Hive sucessfully and consistently produced goodies using a P-less HI/E rxn?  My guess is no...i hope someone proves me wrong

[pancuronium]

Try impurity profiling, assay if available and a different regional strain.
  I have tried to reduce via HI/rP the local ephedra strain here in northern nevada with similiar results.  The work continues...

[halfkast]

Definetly not just in theory man, it's the HI that does reduce it in all the HI methods from my readings.

without working it out myself, I think the equation is about 6HI to 1E isn't it?
So your potentially reduced 1/6th of it, is that right by you?

Gees that was a bit silly wasn't it?  

If I did what you did I wouldn't wash using acetone afterwards because jacked said it removes iodometh, and I'd wanna get high?

[biotechdude]

Definetly not just in theory man, it's the HI that does reduce it in all the HI methods from my readings.

without working it out myself, I think the equation is about 6HI to 1E isn't it?
So your potentially reduced 1/6th of it, is that right by you?

Gees that was a bit silly wasn't it?

If I did what you did I wouldn't wash using acetone afterwards because jacked said it removes iodometh, and I'd wanna get high?

1 ml of 57% HI = 0.99 grams of HI
75 mls of 57% HI was used= (75 x 0.99) = 74.25 grams of HI = 0.5 moles HI

Ephedrine HCl, molecular weight MW = 201.73 grams/mole therefore 0.06 moles of Eph HCL was used

Therefore ratio = (0.5/0.06) = 8.3:1

You believe 6HI 1E is necessary, Swix used 8.3HI to 1E.  So the excess was there, however the decomposition of HI at reflux temps causes the ratio to be lowered and hence slow down/half react the rxn (not to mention side reactions).  This also accounts for the iodine precipitate.

To combat the iodine precipitate, it has been suggested to add sodium thiosulphate or copper filings to clear free iodine, however this will only clear the flask pre or post rxn, still leaving the half reacted goods in there (as the %HI is not kept high enough in the rxn due to decomposition)

So Swix believes that a wet p-less (lets not start on gas phase rxns   ) HI/E rxn is not feasible unless a BLOODY HUGE excess of HI was used (to keep good %HI) and additives were used to combat the decomposition and side reactions.  However, for all that work, i think Swix's mind and wallet would prefer to combat arthritis of the fingers and get mbRP and add that ala

https://www.thevespiary.org/rhodium/Rhodium/chemistry/meth.hi-p.html

On other comments;

Acetone was not added directly as a wash, just a little put in recrystalisation mix.  So it may have removed some iodometh.  However, what does iodo meth/eph look and smell like?  Fluffy white powder or clear crysals?  Remember Swix's 3.5 grams obtained smelt fishy not planty (as plain Eph HCL does) but was definately not meth. 

I have a strong hunch that more than 3.5grams could of been obtained.  Because when steam distilling Ephedra, that is about the ammount of E contained in 400mls of distillate.  So Swix believes that if he kept on distilling the rxn flask; eg 2litres collected he would of had more than 3.5 at the end.  Hypothesising, probably a mix of a tincy bit meth, then maybe equal parts iodometh/eph and eph.

Try impurity profiling, assay if available and a different regional strain.
  I have tried to reduce via HI/rP the local ephedra strain here in northern nevada with similiar results.  The work continues...

Swix is now worried that his Eph could be wack, however where Swix resides Ephedra is very heavily regulated and only has one source (Ephedra Sinensis 3% from China).  It does produce heart-busting fun when had on its own though...  

So is it recommended that Swix obtain mbRP and his pre-made 57% HI and his Eph HCL and give that a whirl.  Are the ratios obtained in Wizard X's

https://www.thevespiary.org/rhodium/Rhodium/chemistry/meth.hi-p.html

suitable?  Or can less be used.  I have UTFSE and have many ratios, but its hard to otain a consistent ratio for pre-made HI, E from Ephedra and mbRP.

[halfkast]

Post 384553 (missing)

(Organikum: "Necessary Concentration of HI ?", Stimulants)
I found this for you, great post regarding the HI SIDE of things.

the proper molar ratio is 2:1 HI:E:P, but the best ratio is 3:1 in a HI reduction with P.

I think your pretty safe trusting WizardX. I had a strong feeling a 6:1 ratio was stated as beeing the amount required for a straight HI reduction.

In any case, you met that ratio and more as you said.

I don't think working with plant extracted E is commonly talked about here, especially with straight HI, I could bee wrong.

If I was using that (the extracted E) I definetly wouldn't have also made so many other changes, because if it didn't turn out as expected I would have the same problem you are now.

I wonder if a % of that plant material contained racemic ephedrine?
Thats been my best guess since last I spoke with you. UTFSE for a post by Aurelius, he compiled a nice big ephedra species list.
Also learn about the typical composition of your ephedra species, thats what I'd do.

You sound like someone with the proper lab knowhow to not spill things on the floor, right?

>>* More/less HI, perhaps it was too concentrated (causing overshadowing side reactions)

Ah, but you determined the concentration volumetrically, didn't you?  

[biotechdude]

You sound like someone with the proper lab knowhow to not spill things on the floor, right?

>>* More/less HI, perhaps it was too concentrated (causing overshadowing side reactions)

Ah, but you determined the concentration volumetrically, didn't you?

 

Swix is young but trained well...although its surprising how much you can learn from home endeavours (eg Chem 101 - dont heat flamable solvent with little flame; burnt knuckles 101, blue-flame floor 101.. haha)

The HI weighed 1.8g/mL and i used 75mLs. That indicates greater than 57% concentration.  But this was at room temp (and 57% is max attainable at 127`c).  And HI gas escaped the flask meaning the maximum (aq) concentration of HI was obtained at that temp. 

Looking up re Ephedra Sinensis; it's alkaloid content is mostly comprised of ephedrine and pseudo-e...so promising there.  It's the main Ephedra specie (also called E.Sinica and a few other names) 

Swix has concluded that a HI and Eph rxn using no P-based recycler is not feasable in a basic clandestine situation.  Others have speculated this, and argued for and against.  But from first hand experience - unless you have a huge excess of HI and was able to combat the HI decomposition and side-rections - it wont work. 

For this unfortunate reason, Swix will regretably go down the mbRP path as Swix doesn't have access to Hypo-P or P-acid anymore. 

This weekend Swix will obtain and extract mbRP; ala SQIDIPPY's numerous threads.  This way, Swix will need alot less HI, and things should go as per established techniques

https://www.thevespiary.org/rhodium/Rhodium/chemistry/meth.hi-p.html

.  Swix will never experiment again (sob..sniffle) ...(hahah, joking)

However, as always, these are Swix's opinions based on Swix's experience.  Perhaps someone else can get this to work; Swix wishes them the best and hope they find sucess and share their experiences.

Will post results from the next MISSadventure (gotta start thinkin' positivly..., Adventure!, Adventure!)

[biotechdude]

Following on from my previous posts...

Swix gathered all his shitty leftovers of ephedra, ephedrine and pseudo; based it all up, and steam distilled to leave 6 grams of ephedrine hcl. 

Swix then bought some match boxes and cut the strips (400 strips in total).  Placed in jar and covered with methanol.  After 20 mins, Swix got gloved up and rolled and rubbed the strips against each other and after much playing, all the RP had came off and the paper was still intact.  RP was then washed in gently boiled methanol, dH20, acetone, HCL acid; a few times and left to dry.  RP had very few specs of paper and felt baby powder smooth and a looked a deep red/purple.  Yield from 400 strips a little over 2 grams final dry product.

HI was made using KI and phosphoric acid.  Basically, equal quantities placed in flask, heated as hot as i could get it, and the HI liquid and gas came over and condensed to a dark red solution.  This was then weighed and concentrated to a density of 1.7g/mL.

These ingredients were placed in a rb flask on an oil bath.  The ammouts were 6g eph, 2 gram RP and 15mL 57% HI.  These were refluxed for 24hrs at a gentle reflux temp of about 115`c in solution.  The solution started dark red and was swirled every couple of hours.  It ended up clear with crystaline skinning appearing on top of the liquid.

The post reaction liquid was diluted with dH2O, washed 2x with NP solvent, based with aqueous NaOH and steam distilled.  Thick oil layer was observed on top of 300 mls distillate.  All the distillate was pH'd to 7 and evaporated at 80`c in open doored oven.  White / clear crunchy powder/crystals were scraped and weighed a tad over 3 grams.

Swix then tried to recrystalise but came a little unstuck.  The product was dissolved in hot methanol and a little acetone added.  Slowly cooled to room temp then covered with ice in small esky and left 8hrs.  Nothing was floating in the cold methanol.  Swix then evaporated the methanal at low temp and revealed 3grams of white/clearish soft crystals (hard to describe).  But not like big solid hard meth crystals (which Swix wants)

Swix gathered his trusted gineau pigs and bioassay was fantastic.  Swix sat in the same spot on his bed with the gineau pigs for 12 hours and didnt move, just chatted our little asses off.  Very clean and nice up, stay up, little waves., then slowly down (2 days later), no crash. 

Swix hypothesises that the mixture was a good mix of meth and iodo meth.  This may account for non-predicted reXtalisation and look of product.  Swix thinks his next batch should be hotter and for longer to push more conversion to meth (and its nice marketable crystals).  Swix would appreciate any input from Bees, regarding his reaction parameters, or perhaps recrystalisation procedure (eg 'dry' his solvent, add less for nano scale etc)

Thankyou

[CainTwister]

1) Steam distilled ephedra to obtain clean white Ephedrine HCl (along with other alkaloid HCL's obv).  [all good]

Did you treat your ephedra with dilute HCl prior to distilling?

[biotechdude]

Ephedra was simply powdered, based and steamed, distillate collected. pH'd, evaporated.

mmm, i didn't wash eph hcl with dilute acid.  I have been curious about pre-base washes though.  Swix uses dry ice and blender; powders it up to lyse cells and release eph inside, but Swix wonders if something else (non-smelly - unlike upon addition of NaOH) could be added to asssist in liberating the alkaloids (and perhaps let sit for a few days prior to distilling)

What % HCL do u add?  Does it make difference to yield?    Any input would bee handy...

And Swix would still appreciate some opinions on reaction time/temp and recrystalisation before his next dream...pretty please?