Author Topic: butalbital / caffeine separation  (Read 2490 times)

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Bwiti

  • Guest
butalbital / caffeine separation
« on: April 05, 2004, 02:52:00 AM »
I've found a product that contains butalbital and caffeine. How could one go about separating these drugs from one another(freebases or salts) - take advantage of solubilities?


heavenadisaster

  • Guest
I asked before...
« Reply #1 on: April 08, 2004, 06:02:00 AM »

Post 447952 (missing)

(heavenadisaster: "isolation of butalbital from aspirin & caffeine", Newbee Forum)


Never got any response though. 

I have a much better idea now I think:

-crush all the pills in basified water and extract with ether(the asprin will stay in the water as benzoate salt, the butalbital and freebase caffiene will go to ether)

-drain off water with asprin, add acidified water(the caffiene will migrate to the water).

-drain water with caffiene, and evaporate ether to recover butalbital.

How does that look?

BieneMaya

  • Guest
have a look at this
« Reply #2 on: April 10, 2004, 01:54:00 AM »
I really don´t know what butalbital is
but I know extraction routes of codeine
that is mixed with caffeine/ aspirine.
 
And codeine freebase has almost the same properties:
bitter taste, insol. in water. Sol in non polar
(Chloroform, DCM, ether and so on).
 
So I think it should work in the same way.
If the stuff isn`t that expensive I would try it anyway.
 
Ok let´s have a look to these codeine extraction:
 
"Can I extract freebase codeine from AC&C tablets"

     Yes you can. but it may be illegal to do so in your area.

     Note: THIS PROCEDURE WILL ONLY WORK WITH AC&C.
     This is a mixture of Aspirin with both caffeine and codeine. These
     are easily available in Canada and the UK. If it has acetaminophen
     in it it will not work.

     Last year someone posted the poor mans guide to Codeine
     extraction. While this helped save the liver of many users, the
     problem was the caffeine remained, and the end product not
     smokable. This guide will show people with some chemistry
     experience how to make smokeable freebase codeine.

     Items needed:
     Aspirin with Codeine tablets. 1000 tabs minimum
     Funnels and filter paper (preferably a Buchner funnel for fast
     filtering.)
     Seperatory funnel.
     Beakers, Evaporating dishes ETC

     Chemicals needed.
     5 % phosphoric acid solution.
     Chloroform.
     Sodium Hydroxide.

     Put tablets in a very large glass bowl and add the hot 5%
     Phosphoric acid solution. The pills will start to disintegrate
     immediately. The reason we are using a 5% phosphoric acid instead
     of just water is so the phosphoric acid will supplement the
     Phosphate in the Codeine phosphate, and to help to increase
     extraction. The reason we are using hot water is to get the most
     codeine into the water quickly. Most of the aspirin will
     precipitate as soon as the mixture is cooled.

     When all the pills have dissolved, stir well, cool your mixture to
     just above freezing. Filter the mixture. When the water has
     drained, take the solids and put it back in the glass bowl. Filter
     the solids three times to ensure that all codeine had been removed
     from the mixture. Discard the remaining paste, as this is mostly
     aspirin, and the codeine is in the water. Note that this step can
     be done in an hour or two with a Buchner or vacuum filter. It can
     take days with gravity filtration.

     You now probably have a large volume of dirty looking water that
     you must evaporate down to a manageable volume of say 100 to 150
     millilitres. Remember that codeine is sensitive to light and heat.
     Codeine sublimates (turns into a gas) at moderate temperature and
     light is known to break it down. This means that care is needed
     when evaporating the water down.

     What you have now is a mixture of codeine, caffeine, some residual
     aspirin and phosphoric acid in about 100-150 ml solution Now comes
     the fun part.

     The next step is to get rid of the caffeine. 1 gram of caffeine
     will dissolve in 5.5 ml of chloroform, but it takes 4.5 Litres of
     chloroform to dissolve 1 gram of codeine phosphate.

     Extraction #1 (caffeine)
     Put your mixture in a seperatory funnel. Wash three times with 20
     ml chloroform. Making sure to shake and vent thoroughly between
     each wash. Remember that chloroform is heavier than water and it
     will be the bottom layer. After the three
     washes you should be left with 60 ml chloroform that has all the
     caffeine from you mixture. This chloroform can be discarded or
     kept if you can recover the chloroform.

     You now have to make the remaining solution in the seperatory
     funnel basic with the addition of NaOH. Bringing it up to 11
     should do the trick. As you add the NaOH you will quickly start to
     see pure codeine freebase start to precipitate out of the solution
     as white crystals.

     Do this right in the seperatory funnel, and please remember to
     shake and vent the funnel thoroughly as many times as it takes
     till there is no more reaction. Don't be too alarmed if the funnel
     get extremely hot due to the chemical reaction, but it may be wise
     to slow the rate at which you are adding the NaOH in this case.

     Remember how above I told you that it took four and a half Litres
     to dissolve 1 gram of codeine phosphate? Now you have pure codeine
     freebase floating around the solution in the seperatory funnel ,
     and 1 gram of codeine freebase dissolves in 0.5 ml chloroform.
     This is 9000 times more soluble than before we added the NaOH.
     With the adjusted PH any residual aspirin is not soluble in
     chloroform.

     Extraction # 2 (codeine)
     Do three 10 to 20 Ml washes with chloroform (remember chloroform is the bottom layer)
     And evaporate in an evaporation dish. The chloroform will quickly
     evaporate and you are left with codeine freebase the bottom of the
     dish.

     Yield: Approx 7 grams codeine freebase per 1000 pills (with 8mg
     C/P per pill)

     Notes:

     1. This is not cost effective for anything less than 1000 pills,
     3000 -5000 preferred.

     2. Several washes of the paste will increase yield. You can tell
     by the colour of the water when you have all the goodies.

     3. Remember that chloroform is a proven carcinogen; so be thorough
     in your work. Make sure evaporation is complete.

     4. DCM can likely be used as a chloroform replacement.

     5. Remember that this process will not work with acetaminophen,
     Tylenol 1,2,3,4 ETC.
     It will only work with AC&C. (Aspirin, caffeine and codeine)

     6. Wear gloves and glasses when dealing with chemicals. Lab safety
     procedures do apply to you.

     7. Sodium hydroxide can burn your dick off.

     8. Smoking codeine freebase can be extremely addictive.

     Grotto.