Almost About to Dream Again (need advice)

[Drug_Phreak]

OK... SWIDP is almost about to dream again… this time with all professional lab glass and equipment. 


Ratios: 7.5g MBRP, 10.2g I2 (close to LG), 10g P-Fed, and 10ml dH20.


Procedure: MBRP will be obtained the usual way (minus the H2SO4 wash) from 35 boxes of matches. I2 will be used directly from the bottle. P-fed obtained from 4 24-pill boxes from a name brand company that has Pseudoephedrine HCl 60 mg, Chlorpheniramine maleate 4 mg, lactose, magnesium stearate, potato starch, povidone, and 17267 different gakks    per pill.

The pills will be extracted with Fester's KOH/Iso procedure. The P-fed will then be recrystallized via STE. 1ml of dH20 will be added to a 100ml RB flask to wet it a little bit. The 10g of P-fed will be added… then 7.5g MBRP is added and mixed in real good. The flask is put into an oil bath and a 300mm Allihn condenser is put on the flask. Flow of ice cold water is started thru the condenser and then I2 is added thru a thistle tube that almost reaches the bottom of the flask. The I2 is mixed around in the flask with a long bamboo skewer gently. Then the remaining 9ml of dH20 is added thru the thistle tube and a flat piece of glass is put on top of the thistle tube immediately after water addition to prevent any HI from escaping. A drying tube with anhydrous CaCl2 is then added. The hotplate is turned on to 25°C... then 50°C... then 75°C and finally 110°C within an hour. It is allowed to reflux for 24 hours @ 110°C (for an inside flask temp of 100°C) and then worked up by Geezmiester’s procedure on Rhodium’s website. The non-polar will be gassed via VE’s CaCl2/HCl procedure. The x-tals will then be vacuum filtered and washed with ice cold acetone. 




1. Have any Bees extracted their feed by Fester’s procedure and then recrystallized by using STE? I would like hear how it went and what the yields where. Especially on name brand pills.

2. Is a 100ml RB flask and a 300mm Allihn condenser too small/short for this procedure?

3. Is it really necessary to do a H2SO4 wash of MBRP? Isn’t an acetone, HCl, and water washing/boiling sufficient?



Do any Bees foresee any major problems with this procedure? SWIDP would really appreciate whatever help/advice/recommendations other Bees can offer SWIDP.

[ChemoSabe]

Ratios: 7.5g MBRP, 10.2g I2 (close to LG), 10g P-Fed, and 10ml dH20.

12.5g of I would be better.

Procedure: MBRP will be obtained the usual way (minus the H2SO4 wash) from 35 boxes of matches.

If extracting RP with methanol it only needs a good tone wash or two after it's free from the strikers and the alc has been decanted. If reusing it it's acetone rinse until it runs clear, an alcohol rinse, a hot dh20 rinse and then a final tone rinse. Sulphuric not needed for either.


The P-fed will then be recrystallized via STE.

Process overkill if you do the deconstruction right. ReX with Geezmeisters Xylene precip technique or simply by dissooving in iso or dH2O and allowing to fully air dry with no disturbance.

If your results from the KOH/alkie boil seem less than stellar then go ahead and STE it but if you follow the plan Fester gives a Xylene precip should finish it up pretty good.

250ml flask might be better in the rxn.
                       
I don't know about that dryng tube you mentioned.

Even after you wash the gassed crystals (it'll bee powder actually) ReXing them is still recommended.

[BullwinkleMoose]

do as ChemoSabe said and increase the I or reduce the E to
maintain the ratio of (1:1.2) for ( E:I ) OK

the moose never does acid washes on his MBRP anymore..
Unless it's benn used a couple of runs and theres gak buildup on the RP


the only thing else that needs to be said is..

Generally you CANNOT trust the labeling of the inactive to be truthfull or complete !

So pick the latest and greatest method of pill
cleaning \extreacting    OK !

[Jade]

P-fed obtained from 4 24-pill boxes from a name brand company that has Pseudoephedrine HCl 60 mg, Chlorpheniramine maleate 4 mg, lactose, magnesium stearate, potato starch, povidone, and 17267 different gakks  per pill.

I don't see how you will get 10 grams out of 4 boxes?

[Apis_dorsata]

you will need a few more boxes of psuedo. swim has been using the koh followed by a ste, and is so very very happy once again. now if swim can stockpile enough psuedo to last awhile, for when the next new gaak hits.

[Drug_Phreak]

SWIDP meant 8 boxes of P-fed. If SWIDP could find a way to get 10g from 4 boxes that would be the best day in SWIDP life.    SWIDP normally obtains MBRP by pouring the strikers in enough acetone and shaking the bottle like crazy very often until all the strikers are white. The MBRP is then covered with acetone and shaken real good for around 30min... then boiled in HCl for 1min... and finally boiled in dH2O for 3min. SWIDP always had good results doing this, but never did a H2SO4 wash and always wondered if it was necessary and also thought that it may actually be harmful to the reaction somewhat. Is it possible that any trace amounts of H2SO4 that stay on/in the MBRP could effect HI generation? Or would the amount (if any) be so low that it would be silly to even think of such things? OK... SWIDP is ordering a 250ml flask instead and they forgot that the Bee on Rhodium's website who did a pic tutorial of a RP/I2 reflux used a 500ml flask and it seemed to climb the flask walls a lot, but since SWIDP is going to use an oil bath this time and not using a FB flask directly on the hotplate like that Bee did they assume that it wouldn’t climb as much. I guess since SWIDP has the solvents to do STE they will do it after the KOH/Iso this time. SWIDP will use Geezmeister’s Xylene recrystallization procedure next time and see how it goes with these pills since that would also save them money on buying solvents. OK... 12.5g I2... cool, that will save SWIDP just enough for another nano. Moose is there currently a better extraction method than KOH/Iso that SWIY uses? If you don’t want to post it on the forum please PM me. OK... Apis_dorsata that’s good to know. SWIDP would love to pile up on some P-fed too at the present time, but 8 boxes of P-fed around here costs them 48 dollars. The P-fed, MBRP, and I2 coming to about $92... actually not too bad for 8g of crystal. It goes for $100 a gram or more here. SWIDP is going to try the Ma-Huang extraction again once they get better equipment to do so. I’m sure you’ve seen a drying tube like this before...

.

I probably should have said that the drying tube was put on top of the condenser.


Thanks everyone!!!

[BullwinkleMoose]

your on it dude !
that'sthe latest out here !

[ChemoSabe]

I think I cross associated memory of this

Post 483763

(mr_pyrex: "Regarding drying Acetone by way of CaCl....It...", Stimulants) with your mentioning of the CaCl drying tube.

Swim's buddy used to use a 300mm Alihn topped with a 200mm lickbag (both 24/40) topped with a stopcock adapter capped with a 7 meter length of vinyl tubing leadng outdoors. The cooling system for the condensers was a small fan. No water was needed. 250ml 24/40 erlenmeyer sitting straight on the hotplate for a similar rxn. Always worked with never a fuckup. Swim's buddy hates oil baths so avoids them whenever possible.