Ph control when gassing product

bio · Working Bee

BP of azeotrope,C Composition ,wt % Water other componentnt

Toluene 84.1 13.5 86.5

Ethylbenzene 92.0 33.0 67.0

m-Xylene 92 35.8 64.2

O & P xylene are almost the same as the M isomer. Ethylbenzene is cheap.

64bandil · Busy Bee

I usually use 30% hydrochloric acid dripped in slowly...

joe_aldehyde · huxleys associate

ok so what about adding too much dilute hydrochlorid acid, will it fuck everything up? not talking about H2SO4 - that sure fucks everything up Smile

swims pretty interested in amphet-amine phosphate, since he believes that the anion of the amine salt really makes a difference in terms of pharmacological quality. and sulfate isn't as common in ones' body as phosphate is (does anybody know what adenosine-triphosphate is Wink

even stranger the fact that swim got amphet-amine sulfate solution from 2 different places (official ones so it was legit. amphe-tamine) and there was QUITE a difference in the effects. the second one was MUCH more mellow and produced heavy body load. really strange since the "recipe" was the same, with citric acid as buffer, sugar as sweetener (yadontsay!!) and k-sorbate as conservant.

bio · Working Bee

.......ok so what about adding too much dilute hydrochlorid acid, .........

After you isolate the amine and calculate the amount of HCl needed if your amine isn't relatively pure then too much HCl will have been added. A small ampunt of excess HCl will not damage anything and it will leave along with the water at the azeotropic temp (108deg 21%) if it didn't mostly escape as the gas before

If you are unable to get concentrated HCl I would be surprised. The more water
that must be removed requires more xylene for example. There is a large excess of solvent used in this procedure. Look at the azeotrope data I posted and WORK IT OUT, then you will know exactly how much water is removed at the azeotropic temp by a given weight of solvent, then add a healthy excess. Using bandils ratio of water to solvent would be wise.

Neighbor Joe did this method a couple times with toluene and it works very well. Takes a longer time though than extracting with aqueous HCl which is what Joe usually does, however he told me that you need CLEAN amine so it doesn't turn into a gummy mess.

joe_aldehyde · huxleys associate

bio,

it doesn't require more xylene but just more time if you use a water trap and don't evaporate it. if you meant swim, he can get huge amounts of HCl cc.
he wonders how he can get clean amine without distillation, since the amounts he is about to work with are quite little. repeated A/B will help, yes?

bio · Working Bee

......he wonders how he can get clean amine without distillation, since the amounts he is about to work with are quite little. repeated A/B will help, yes?.........

Yes, it can be done. Skip the A/B as you will lose too much with small amounts. Excessive brine washes with steaming and aqeous extraction will do it, pm me if you want.

riggie · Fri Jun 24, 2005 6:10 am

I just used toluene or ether, sure dried it before, but forgot once. what happend was that first a layer formed at the bottom of the glass but as I kept adding hcl gas, big crystals started to form and evntually I got clean product.
Be carfull not to overgas have some amine by hand to add if it happens. I always have a ph meter in the solution and add hcl gas carefully.

pekebaz3 · Wed Jul 13, 2005 1:27 pm

here is that link

https://www.synthetikal.com/hiveboard/newbee/000513755.html

was wondering if someone could help me calculate the molar amount for mdma.fb and 31% hcl acid.(should I dilute this with dh2o to get 10%?)for this.any help is really appreciated.thanx
I really just need the molecular weight of mdma.fb
I found the one for hcl.but I've read that they different and can't seem to find it.thanks

joe_aldehyde · huxleys associate

if you have the structure of mdma fb, go ahead and keep adding the atoms' masses.

bio · Working Bee

Google on this pekabaz3;

EniG. Chemistry Assistant version 2.4

It's a freeware solution and mole calculator that's real handy and easy to use. No sustitute for understanding what you are doing though. It has all the formulas as well to help you understand what is being done for solution calculations.

For some f.........g reason I can't figure out how to add chemicals to the existing library. The instructions are all there but I can't figure it out. You will love this thing and if you do figure out how to add to the chem list please HELP ME!

Also I would use concentrated HCl as it's mostly water anyway so why add more water when you are trying to remove the damn stuff! I did it this way a couple times with bandils procedure which works quite well but is too much hassle IMHO, at least when using clean fractionated amine it can be dried with solid KOH or NaOH very quickly.

pekebaz3 · Thu Jul 14, 2005 1:14 am

thanks for that progie...I found one online but it didn't have that many features on it.I still can't figure out the freebase form..this is the hcl salt of it. C11H15NO2
I'm still pretty new at this so please be kind.I'm probably just going to use that formula for the reaction.just make sure to use a little more hcl then needed.
thanks agains

also:can someone tell me if yields are usually the same for this azeotropic reaction as with hcl gassing?thankyou

bio · Working Bee

Look, just add it up. HCl is 36.46 so this subtracted from your salt is the base! There is no Cl in your empirical.

If there are 2.4moles base amine it needs 2.4moles HCl which is a gas. Don't quess and if you add too much then a host of other problems will occur. A very small excess can be used say 1-2% assuming that the amine is pure and you are not weighing contamination. So better to titrate or take more than one crop.

The solution calculator (little beaker button) will give you g/L, % and molarity. The formulas are in the bottom window so make sure that you do them by hand until you know WTF you are doing.

pekebaz3 · Thu Jul 14, 2005 12:59 pm

ok..I did some quick math and hope someone could tell me if I'm heading in the right direction.
molecular weights
mdma.fb-156.7823
hcl-36.461
ok.so if I have 40g of my amine, then that is .255 mole.
then .255*36.461 is 14.44g.so that's the amount of hcl.but I'm not sure how to calculate the weight with the water.do I multiply h20's molecular weight(or 2x it's weight becuase it is 31%hcl) by .255 and add that to the weight of the hcl to get the total?might seem stupid but I'm struggling with it.thanks for everyone's help.

hAzzBEEn · Thu Jul 14, 2005 9:32 pm

3,4-methylenedioxy-N-methylamphetamine, C11H15NO2 (mol. wt. 193.24) from Lycaeum

So, 40g isn't .255mol, because the mw is NOT 156.8.
BTW .255*36.461 is 9.30, not 14.44.

MDMAFB at 193.24g/mol... 40g/193.24g/mol = .207mol
HCl at 36.461 g/mol... 0.207mol*36.461g/mol = 7.547g

Solutions designated by % are {weight of solute(HCl) / weight of solution(HCl+H20)}
(%) = (g HCl) / (g HCl.aq) ==> (g HCl.aq) = (g HCl) / (%)
7.547/.31 = 24.35g HCl.aq, so you need 24.35g of 31% HCl Solution

A quick Google search found Re: Normal vs. % HCL in a solution with the needed info.
A quick Google also found the image, molecular weight, and chemical formula at the top of this post.

Good luck.
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pekebaz3 · Fri Jul 15, 2005 1:36 am

thanks for the help.