The Vespiary

The Hive => Newbee Forum => Topic started by: BieneMaya on January 19, 2004, 05:36:00 PM

Title: gasing with HCL in IPA
Post by: BieneMaya on January 19, 2004, 05:36:00 PM: Has anyone experience with that gasing method?
The HCL/IPA solution is made via gas generator first.

https://www.thevespiary.org/rhodium/Rhodium/chemistry/hclgas.argox.html (https://www.thevespiary.org/rhodium/Rhodium/chemistry/hclgas.argox.html)

Then one has just to react that reagent with your free base.
The main advantage is that the HCL/IPA could be stored.
Title: High Biene Maya! I´ve heard from many sides...
Post by: Xicori on January 19, 2004, 05:57:00 PM: High Biene Maya!

I´ve heard from many sides that this works nice, but i haven´t tried it yet.

Just make sure that your IPA is anhydrous, and chill it before gassing.

SWIM prefers to mix the (distilled) freebase with IPA, add aqueous HCl until pH is slightly acidic and then add Et₂O to crystallize your salt. - worked like a charm ;)

best wishes,
xicori
Title: i will try MeOH with HCl...
Post by: methlab on January 19, 2004, 07:36:00 PM: i also want to store the HCl(g), cause my gasing apparatus is not very good. I will lead anhydr. HCl(g) into dried chilled MeOH. Give me a couple of hours and i will tell you if it works, greetings :)
Title: Hoi Xicori! Yes of course you IPA or any other
Post by: BieneMaya on January 21, 2004, 03:16:00 PM: Hoi Xicori!

Yes of course you IPA or any other liquid you want to
react HCL with MUST be anhydrous.

I heard of your method too but I have no diethyl ether right now. But someone told me DCM can do the same job
however with poorer result.

I will give it a try with IPA when I have time and tell you the result then.

Hey Methlab!

Do you have any results for us now?
Title: DCM replacing ether.
Post by: terbium on January 21, 2004, 04:14:00 PM: heard of your method too but I have no diethyl ether right now. But someone told me DCM can do the same job
however with poorer result.
Probably a much poorer result.
Title: Biene, i dont think that HCl in IPA without...
Post by: Xicori on January 21, 2004, 08:49:00 PM: Biene, i dont think that HCl in IPA without Ether is a good joice! - Most of our beeloved amine salts are more or less oluble in IPA, so you will loose some product here!

It would be better to dissolve the freebase in Toluene or Ether (if you can get some, but Toluene/Xylene might work good too!), and then add the HCl dissolved in IPA until no more crystals sprint to live!

best wishes,
xicori
Title: Thanks Xixori, Yeah that are great news that...
Post by: BieneMaya on January 22, 2004, 03:33:00 PM: Thanks Xixori,
Yeah that are great news that xylene works too.

However I don´t want mdma freebase to convert into a salt.
Oxycodone freebase is my target.
But it´s an amine anyway.
So the solubility of its salt in IPA isn´t a big difference, I think.

I guess the xylene must be damn anhydrous as well, doesn`t it? Or is it a problem to use 99% xylene?
Title: I've done that using 99% by volume otc IPA.
Post by: scram on January 22, 2004, 06:23:00 PM: I've done that using 99% by volume otc IPA. Acutally I've found that the density of IPA sold as gas line dryer is a slightly higher density than the 99% by volume IPA sole in the pharmacy. Should be more water in the Pharmacy IPA if it's by volume. I would stay away from the gas line dryer ipa because it just has some odd additive scent compared to 99% or lab grade anhydrous IPA. I used a 1/2 gallon garden sprayer loaded it w/rock salt and lab grade h2s04 and gassed @ -10c to 0c. It took quite a bit of time to do even with stirring. I still to this day don't know exactly the concentration it held.

"America, the land of Big burgers, Big ideas, & big fat glutenous motherfuckers who who eat up everything and plug up the sewer lines"
Title: So stirring of the IPA is absolutly necessary.
Post by: BieneMaya on January 23, 2004, 02:40:00 PM: So stirring of the IPA is absolutly necessary.
I thought it could be done without stirring
since I have only one mag stirrer.
And that one should be used to stirr the H2SO2.

But how much stirring is necessary of the IPA?
Maybe a light hand stirring with a magnat
from time to time can solve this problem too.
Just a thought.......

Otherwise I must buy another mag stirrer.
Title: Gas absorption bottles.
Post by: terbium on January 23, 2004, 05:49:00 PM: I used to have some tall, narrow bottles that I would use for absorbing a gas into a liquid. I think that they were called specimen bottles - clear flint glass, the opening tooled for a large rubber stopper, available in sizes from 250 ml up to a couple of liters. The narrow profile gave the gas plenty of contact time with the liquid, even without stirring.
Title: gaswash- bottles?
Post by: BieneMaya on January 23, 2004, 07:23:00 PM: Yeah I have some gaswashbottles here.

I think that are the ones you mean.
5cm diameter and 20cm tall.

Ok I´ll give it a try.
Title: swibbs done it
Post by: barkingburro on January 27, 2004, 08:27:00 AM: this is actuall y swibb's preffered way of gassing assuming he feels inclined to do so. keep carefeul measurments of the ice cold ipa before and after dissolving the gas. too much hcl is a always a bitch, and there is loads of fumes too. also bring the solution of fb/meth and xyl + hcl and ipa to 110 deg C to boil off all of the ipa. mmm
crunchy
Title: heats up
Post by: Grouch on April 18, 2004, 05:04:00 AM: If you can, try to keep the IPA cold while gassing because it tends to heat up during the gassing. My friend used to put the 4L bottle of IPA on a scale and keep note of the mass of the HCl/IPA sol'n. You will see when it stops climbing.

The IPA holds the HCl very well. There was barely any fumes coming out while gassing.

HCl will not go into DCM, barely.
Title: Contents of the bubbler?
Post by: biffman on April 20, 2004, 09:38:00 PM: One thing that I did not see mentioned on Rhodium bubbler setup is what is the liquid in the bubblerthat is before the trap and the reaction vessel?
Title: It´s H2So4 again. You need it to dry the ...
Post by: BieneMaya on April 20, 2004, 10:47:00 PM: It´s H2So4 again.
You need it to dry the formed HCL.
Otherwise it could have some water in it.

H2SO4 is a good drying agent in in gasing setups.
It pulls all the remaining water out of the gas
to form a diluter sulfuric acid.
So in this case a strong conc. sulfuric acid is needed.