Author Topic: RP / I / GAA  (Read 6102 times)

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Coitus

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RP / I / GAA
« on: February 22, 2003, 03:54:00 AM »

The dreamer started with approxamately 12.5g freebase psudo extracted from several boxes of 96ct red hots. (soaked in tolune a few days, discarded then boiled in tolune, dryed, waterless a/b into tolune then evaporated)

This was casually tossed into a 250ml boiling flask along with 7g fresh lab grade RP. Then 3 mls of DH20, and 5mls of GAA was added and mixed throughly. Condensor was then attached and cold water was started. 2g of lab grade resublimed I2 was added thru the top of the condensor.

No visible signs, so the temp was brought up to approx 115F when it started. flask filled with swirling white smoke and reacted for a few minutes. Another 2 g of I2 was added and similar reaction took place. This continued until a total of 18G of I2 was reacted. (Took about 20 minutes total) A 1-holed stopper was then added to the top of the condenser with some aquarium tubing going out the window.
The temp was taken up slowly, due to violent bubbeling and swelling up to 5 times the original mass of starting material. About 45 minutes later, the temp was stabelized at 200F for approxamately an hour. The reaction appeared over, but I wasn't buying it that quick. The temp was then gradually brought up to 300F and was reacting and refluxing beautifully. This was then left for 1 1/2 hours. Upon returning, the dreamer noticed the mixture had turned much darker and was refluxing 3/4 the way up the condensor. Just then he also noticed the teflon on the pan holding the oil appeared to be shedding and exploding in the oil, and it was scaring the shit out of him.
(Damb, that was the only pan the bitch left me)

Dh20 was then added thru the aquarium tubing to wash any escaped goodies back into the flask. when the h20 hit the flask, a small reaction of foam and bubbles was noted. water was added till it looked like a 2 to 1 ratio of water to reaction mixture. a little heat and mixing then filtered the RP, rinsed the flask and the filtercake with tolune. an equil amount of tolly was added, then shook violently and poured into a sep funnel. It was left for 20 minutes, then the tolly was discarded. 2 more of the same tolly washes later, several grams of lye was added to the mixture. (I couldn't believe the amount I had to add to get the test strip over 10) It was then shaken with an equil amount of tolly and left for 20 minutes to seperate. Moved the tolly to another sep funnel and added another equil amount for a second pull. Thru a couple more grams of lye in there for luck and seaparated as before. The 2 tolly pulls were then shaken with a clean DH20 wash that came out looking real clean. More dh20 was added with approxamately 2mls Muriatic acid, shaken, seperated and deposited in a pyrex plate in the toaster oven at 200F

About 5 Grams of beautiful white crystals was scraped from the plate after evaporation. Another pull on the tolly netted another 2 grams. and the 3rd pull is gonna sit for a couple days before yield is known.

Bioassay is the best shit this boy has hit in 2 years. (same amount of time his glassware and apron was in cold storage)
    
Yee-Fucken-Haw (Damb, the suns coming up quick)



Spun1

  • Guest
Interesting data
« Reply #1 on: February 23, 2003, 05:30:00 AM »
SWIS did a rxn with just GAA no H2o and had rather impressive results just not that great of a yield. The ratios SWIS tried were probably the reason for this. But SWIS has read that when H2o is added to a rxn with GAA that it makes more Hydriodic or something to that effect. Will have to do some more research on this..Thanks for sharing your experience


wareami

  • Guest
Impressive
« Reply #2 on: February 23, 2003, 11:14:00 AM »
When Ibee first read this, he was a tad confused about the GAA! Just so no newbees fall out the back of their honeycomb, Ibee would like to clarify.
GAA= Glacial Acetic Acid Correct?
Rather than ask what purpose this serves, Ibee would rather read further! But enlightenment is always welcome coming from the DoBees currently researching this method with the addition of a new substance!
Very Nice write-up!
Thanx Coitus
Peace of the reaction

Have FUN-Bee SAFE



Rhodium

  • Guest
GAA
« Reply #3 on: February 23, 2003, 11:44:00 AM »
GAA = Glacial (100%) Acetic Acid

For its purpose, read the references in

https://www.thevespiary.org/rhodium/Rhodium/excellent.ideas/


MnkyBoy78

  • Guest
It does work
« Reply #4 on: February 23, 2003, 02:39:00 PM »
SWIM has used GAA in many of SWIM's rxn's (hypo/I2/E/GAA).  Seem to remember SWIM saying that w/ 4 ml of hypo, ~10 -12 ml of GAA was added.  But in SWIM's storie, the e and I2 were mixed/chilled.  The hypo was then added.  After the bubbling ceased, and before the vessel went onto the heat, the GAA was added.  After ~6 hrs of refluxing, 2.5 ml of dh2o was added.  It was noted that the contents turned a milky color along with the evlolution of white fumes.  (Presumably the milky color was the HI in the solution).  Bioassay revieled it was good, but the stench of cat-piss/vinagor is a main factor in the wrather to use GAA in the rxn.

Nice write-up though


ballzofsteel

  • Guest
Clue?
« Reply #5 on: February 23, 2003, 03:10:00 PM »
Ive asked before but...
Can anyone tell me why GAA is the favoured solvent for this rxn,and/or the way in which it influences the rxn,
besides saying,"Thats how they did it,and it worked well,so it must be good"???

Is it a gravity/density/solubility issue?
Does GAA only function as a solvent in this rxn?
Does it serve as a buffer?

Ive seen refs mentioning its use in waterless HI production,as this is were my questions stem.

Would appreciate the input.

Good work dude. :)

fierceness

  • Guest
i believe it increases the concentration of HI
« Reply #6 on: February 23, 2003, 03:47:00 PM »
i believe it increases the concentration of HI above its normal 57%

felon

  • Guest
rp/i/gaa
« Reply #7 on: February 23, 2003, 05:46:00 PM »
If you like the results from this reaction I have another you might like.  Try using DMSO when you make your HI.  The paticular one I have tried involves 43g of sodium Iodide dissovlved in 100ml of dmso. To this add 8ml of sulfuric acid. After it reacts filter out the solids. Voila you have some HI. Im not sure of the exact%, maybe one of the pro can figure it out for us, but i believe it to be more the 57% as it reduces an has no need for RP

;)

Rhodium

  • Guest
Sulfuric acid oxidizes HI to I 2 .
« Reply #8 on: February 23, 2003, 06:23:00 PM »
Sulfuric acid oxidizes HI to I2. Bad procedure.

VideoEditor

  • Guest
writeup comming
« Reply #9 on: February 23, 2003, 06:39:00 PM »
You all must be reading my mind. I will be posting the "Long Wet Reflux in Less Time" soon. It uses GAA but in a slightly different way.  Instead of just replacing or simply adding GAA to the water what I will propose is this:

Turn the psuedo freebase into an ester. React the ester with HI. Initial tests show very clean rxn with good yeilds and it finishes in under 8 hrs.  Bio assy suggests same gogo as a 30 hr reflux but much more data is needed to make any claims. Schedule permiting will post writeup soon.

peace -VE


SPISSHAK

  • Guest
I don't think that would be worthwhile
« Reply #10 on: February 23, 2003, 07:04:00 PM »
The only thing that would happen is that you would make an ester, on addition of excess strong acid (HI, H2SO4, whatever)and heat you just get hydrolysis back to acid and amino alcohol.
A total waste of time.
If you look at how this was originally done in the '80s they used carbondisulfide, HI, and red phosphorous.
The carbondisufide solvent was ideal since it dissolves Red phosphorous.

Coitus

  • Guest
psudo Ester??
« Reply #11 on: February 23, 2003, 07:13:00 PM »
I never even thought of trying the ester..........


I guess I assumed it would be converted in to some type of ester when I mixed the freebase with the GAA and RP??
I know....assuming anything isn't a good idea.....
The main reason for trying this was to bring the concentration of HI up without worrying about an RP flash fire.

I do belive the concentration was very high due the the amount of smoke coming out the 15 foot aquarium tubing that was attached to the condensor. 



I was able to snag a couple more grams on the 3rd pull,
I believe yields suffered due to only running a few hours.
I'l be busy for a while, but may try running one for 6 hours next time. (After getting a deep fryer or better pan)

later,



VideoEditor

  • Guest
With all due respect....
« Reply #12 on: February 23, 2003, 07:49:00 PM »
With all due respect SPISSHAK I beelieve your wrong. SWIVE is certainly no chemist by any means so I can't explain the exact mechanics at work here, but this total waste of time just dreamed some of the best gogo SWIVE has ever dreamed, in about 1/3 the time.

-VE


Organikum

  • Guest
Carbondisulfide
« Reply #13 on: February 23, 2003, 09:27:00 PM »
dissolves red phosphorus? I have no MERCK on this computer but as I remember carbondisulfide dissolves white phosphorus but not the red.
But I would love to get proofed wrong on this.

ORG


Rhodium

  • Guest
Red P is only soluble in PBr 3 .
« Reply #14 on: February 23, 2003, 10:18:00 PM »
Red P is only soluble in PBr3.

SPISSHAK

  • Guest
No offense taken here
« Reply #15 on: February 23, 2003, 10:42:00 PM »
Video editor I may be wrong so if your scheme is workable, by all means let us know how you genrated the ester, and how you isolated it for reduction.
And how well the reduction went.
I'm all ears.

Osmium

  • Guest
> With all due respect SPISSHAK I beelieve...
« Reply #16 on: February 24, 2003, 02:13:00 AM »
> With all due respect SPISSHAK I beelieve your wrong.

I fail to see the advantage of preparing an ester.

> I do belive the concentration was very high due the the
> amount of smoke coming out the 15 foot aquarium tubing
> that was attached to the condensor. 

I don't think that HI will be soluble to the same extend in acetic acid as it is in water. If big quantities of HI were given off by the reaction you added too much I2, so less should work in the future. I'd rather use more solvent though and keep that healthy excess of I2 as it is. Also, the amount of water added was on the low side, it was most likely all consumed by the time you added the last portion of I2.


SPISSHAK

  • Guest
No Osmium
« Reply #17 on: February 25, 2003, 10:13:00 AM »
I made no statement that there was any advantage to preparing an ester and subjecting it to treatment with a concentrated acid and heat, you merely get back the carboxylic moiety, and the amino alcohol. I think you were thinking of someone else, in principle esters are easier to reduce than alcohols but that depends on the method of reduction.

fargo

  • Guest
So thirsty for more on this one...
« Reply #18 on: February 15, 2004, 03:47:00 AM »

Organikum

  • Guest
question to Osmium
« Reply #19 on: February 15, 2004, 02:20:00 PM »
How do you come to believe all the water was used up at the end? The reaction produces its own water IMHO by:
ROH + HI = H2o + RI
Is this wrong?
And if so, why?

Also wouldnt PI3 be formed if not enough water is present the PI3 being well suited to iodinate the benzylic alcohol?
2P + 3I2 = 2PI3
PI3 + 3ROH = 3RI + H3PO3
(PI3 without water, a standard procedure for iodinations avoiding subsequent reduction by HI, PI3 being a stronger iodination agent as HI btw.)

For following reduction HI is needed, no question and for this to form some water.

I agree that the addition of iodine was done to fast and in to much at once as only so much should be added that a white fog appears over the reaction - thats enough - more is waste..

Great writeup btw.