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Recrystallizing Freebase Pseudoephedrine (by Geezmeister)
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tina_craig

Joined: 07 Feb 2005
Posts: 26
642.42 Points

Wed Feb 09, 2005 10:48 pm
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One way to do this is by boiling the freebase crystals in distilled water, but do this in a flask with a condenser, since you will lose freebase pseudo in the steam that boils off. Using a condenser limits the pseudo loss. Bring the water to a boil. During the time it heats up the crystals will dissolve, then reform at the top of the water. You can filter them out and rinse with dH2O to clean. The water will be filthy.

The other way to recystallize is to redissolve them in hot solvent, such as naptha, filter, and chill the naptha. You will have some yield loss as even room temp or cold naptha will hold some freebase pseudo. You can gas or titrate the solvent for the rest of the pseudo.


Last edited by tina_craig on Thu Feb 24, 2005 1:49 am; edited 1 time in total
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java
Consumer
Joined: 07 Feb 2005
Posts: 736
Location: The Mexican Republic
21796.14 Points

Wed Feb 09, 2005 11:26 pm
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Quote:
will lose freebase pseudo in the steam that boils off.
you may ask why....it has something to do with azeotrophes

...."In chemistry, a mixture of liquids that has a constant boiling point because the vapour has the same composition as the liquid mixture. The boiling point of an azeotropic mixture may be higher or lower than that of any of its components. The components of the solution cannot be separated by simple distillation.

First, an azeotrope is best described as a constant boiling blend. To be an azeotrope, the material has to be a mixture or a blend of at least two different elements or compounds. For example, "neat" nPB is not an azeotrope because there's nothing else in it but molecules of nPB. Bromothaneô R is a mixture of nPB and isopropyl alcohol. So Bromothaneô R could be is azeotrope.

Now let's consider the boiling point of these materials.

The boiling point of nPB is about 70? C/170? F. But mix nPB with a small but precise amount of alcohol and the boiling temperature suddenly drops. This is very odd and unexpected. The two chemicals are still separate and distinct in the mixture; there has been no chemical reaction in which they actually change their chemical state. But somehow the two chemicals are working together to lower their combined boiling point. And, most importantly, when we boil some of this mixture in a beaker the two constituents will boil off at the same rate.

Let's suppose the mixture we are testing is 97% nPB and 3% alcohol. If we measure the vapors coming off the boiling liquid, we would be pleased to notice that the mixture of vapors also was at the same 97:3 mixture. When we chill those vapors and distill the material, it again will have the same 97:3 mixture. In fact, no matter what we do the mixture it always stays at the 97:3 proportions. This means we have created an azeotrope"

......curtesy of http://12.162.180.114:90/synthetika/azeotrope.html and the Watcher
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geezmeister
Busy Bee
Joined: 07 Feb 2005
Posts: 22
1066.24 Points

Wed Jun 22, 2005 9:47 pm
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The azetrope of pseudo and water contains only a small amount of pseudo. Steam distillation of pseudo takes a lot of steam, and leaves you with pseudo mixed in a lot of water. Separating the pseudo from the water efficiently enough to obtain a high yield of the pseudo, and getting enough of the pseudo to steam distill over in a reasonable amount of time was always a problem that hampered the effectiveness of steam distilling pseudo.

Given the effectiveness of the current foilants in pillstock, perhaps it is time to revisit steam distillation.
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