Author Topic: Short Questions Thread  (Read 10820 times)

Terror

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Re: Short Questions Thread
« Reply #1060 on: October 14, 2011, 07:04:10 AM »
I think he means extract the salt from the hcl with dcm.. therefore extracting rather than washing.. language barrier maybe? I'm not sure about the migration of a red color though, didn't experience it....

My assumption is that MD a hcl is liberated from the hcl into the dcm, the dcm slowly evaporated to produce clean crystals... does that sound right? I'm not sure where to go from here, ie the dcm extract route or to evap the hcl layer then clean the MD a hcl via acetone...

Does my hcl mdma hcl layer sound like things look right?
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RoidRage

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Re: Short Questions Thread
« Reply #1061 on: October 14, 2011, 07:13:41 AM »
Your assumption is flawed since MDMA HCl is for sure a lot more soluble in water than in DCM so it's would be pretty much ineffective at extracting and would takes many many extractions to get an appreciable amount. I'm pretty sure he was talking about washing.

Just curious...Why not simply evaporates your water layer ? Wash it with DCM if you want though ;D

I've reread sassa's post, and he's really implying he's washing the aqueous layer, not extracting like you pretends. He uses it to get rid of the red color. If he used it to extract too, he would carry over the red color which is exactly what's he trying to get rid off ;)

Terror

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Re: Short Questions Thread
« Reply #1062 on: October 14, 2011, 07:39:28 AM »
Sedits comments led me to that conclusion. My acid layer is clean white, no red at all anyways.. I didn't consider the solubility levels of the dcm / water...

 I was hoping for dcm as the evap level is far less than water, obviously... what's the best way to evap the water layer then, slow distillation or just chuck it on something warm? Fan drying a water layer makes me think this will take forever......
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RoidRage

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Re: Short Questions Thread
« Reply #1063 on: October 14, 2011, 05:35:55 PM »

 I was hoping for dcm as the evap level is far less than water, obviously... what's the best way to evap the water layer then, slow distillation or just chuck it on something warm? Fan drying a water layer makes me think this will take forever......

Fan drying isn't that long, even for medium-sized batches. If you're in hurry, you can reduces the water volume in vacuo or at medium heat on a hotplate. All of this works well

Terror

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Re: Short Questions Thread
« Reply #1064 on: October 14, 2011, 08:50:58 PM »
What method ? He's simply extracting the MDMA freebase from the non-polar solvent with acidified water. While not being an actual titration, it's what people call the ''titrating'' as opposed to gassing. A correctly-done titration requires drop-wise addition of acid to neutralise the base while constantly reading pH to know when all the freebase has been neutralised (converted to the salt). I haven't calculated it, but target pH is probably about 3-4, and not 7, since a weak base is being neutralised by a strong acid. Once you overshoot with HCl , pH immediatly drops to 1.


Well, I based on that I can conclude a 5% hcl wash is too much hcl.... my water + product layer Ph test shows 1.... is all hope lost here?
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RoidRage

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Re: Short Questions Thread
« Reply #1065 on: October 14, 2011, 09:32:57 PM »
It doesn't really change anything beside having a shitty color (which can easily be cleaned by anhydrous acetone washes and recrystallisation as I already stated). I had problem having the salt crystallising once because of high acidity (I've read somewhere on here that it interferes with crystallisation). It doesn't really affect yield either.

Don't worry, your product is in that aqueous layer  ;D

« Last Edit: October 14, 2011, 09:59:13 PM by RoidRage »

Terror

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Re: Short Questions Thread
« Reply #1066 on: October 14, 2011, 10:33:23 PM »
You just made my day! Will report back when evap complete, thank you sir!
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Wizard X

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Re: Short Questions Thread
« Reply #1067 on: October 14, 2011, 10:50:18 PM »
This attachment will help understand extraction via solvents.
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sassa

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Re: Short Questions Thread
« Reply #1068 on: October 14, 2011, 11:06:25 PM »
Well....yeah like people said here,there is nothing new here,not any "sassa´s method" at all please!.the DCM wash of the acid water layer that contains the mdma.HCL or mda.HCL it´s for get ride off the intense colour the water layer usual presents on my extractions,posibly because i use and hcl excess with good amount water to make sure all mdma or mda migrates to the water layer.I used once to titrate  exactly to ph 5-6 but to me it´s more tricky and time consuming.
   Of course,if your water layer it´s clear not wash at all.Mine it isn´t,so if i don´t make that wash,i will need more acetone washing or recrystallization.Anyway,the product will be finally very clean.l
   About that colour of the acid water layer that contains mdma,i don´t know since the begining what causes that.... but sure colour and intensity changes with hcl amount used....less hcl...orange/pinky water layer.....good excces:blood red,violet,......I suposse now t´s related to a little amount free amine because too much free hcl floating around????....if it´s that,you guys are right when say i´m losting i tiny amount of mdma on that DCM wash.It´s all about time!...with my hcl excess i need that to get crystalls that are clean enough to make a single acetone wash and go directly to storage.
   About mdma solubility on DCM i can´t show technicall data,but by bad experiences,i know gassing hcl on DCM when the salt it´s mdma doesn´t work!...posibly little solubility  of mdma on DDCM andcombining  little traces water with hcl floating around....Fuck up the crystallization way easier than on toluene....but gassing for MDA on DCM yeah it´s so easy it´s pleassure....so i think mdma it´s little soluble on DCM  but doesn´t MDA.
  And finally,the best method to evaporate the water layer if it´s acid like mine it´s a fan blowing directly over the water surface making turbulence,with the water layer on a flat crystal pan....I finished yestedary a batch that resulting on 500 ml water layer....today after 24 hours excactly,i have only litle wet crystalls,one day more will be ready to acetone wash.It´s the faster method i think.Remember cover hotplate stirrer,vacumm pump,....with plastic bags if are on same room....i´ve ruined one stirrer and  pump because that...oxidation hurts!!.
   The evaporation it´s quickly and you will finish with a crystal cover surface and water on the bottom that seems don´t want to evaporate....when i arrive to taht point,i scrape that crystall surface,stirr the crystalls with the remaining water and put againg the fan near....repeat that after you are sure the crystalls are dry.....and finally ...when you think they are dry....put under a low heat source(like a 60 w bulb) for one hour to dry it completly...that will make the finish acetone washing not take a lot of salt disoled on little water pressent.....and that´s all!.....
  PD:we all have our "methods"...posibly lesrned by mistaking....so that isn´t a method at all..it´s the way i do things i works fine for me 8)

RoidRage

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Re: Short Questions Thread
« Reply #1069 on: October 14, 2011, 11:17:16 PM »
Thanks for the clarification sassa 8) :)

sassa

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Re: Short Questions Thread
« Reply #1070 on: October 14, 2011, 11:25:40 PM »
And one final thing about method we are talking about latelly.....i was thinking since time ago on check it out an experiment to reduce evaporation time.Please tell me what  you think.
1.   After extracction i finish with 500 ml acid water layer containg mdma hcl disolved.
2.   Neutralize acid excess with baking soda:so big gas evolution,NaCL formed but disolved on the water and when ph  reaches neutrality,posibly little bicarbonate begins to precipitate.So filtering the water layer to get ride of bicarbonate.
3.evaporate under heat and vacumm until dry resulting on :MDMA HCL +GOOD AMOUNT NACl
3.Put minimum warm methanol to disolve the mdma hcl,and supossed the nacl will stay undisolved mostly?????
4.Filter,reduce methanol by slow boiling until crystal formation,adding acetone until crystalls snow from solution again.
...If that works...can be as fast and clean as gassing.....
    What do you think ?.......the problem it´s about solubility NaCL on methanol...posibly another alcohol will be better choice,,,anyway....litle Nacl on the finall product it isn´t nothing too much bad....


Terror

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Re: Short Questions Thread
« Reply #1071 on: October 24, 2011, 07:27:34 AM »
New questoion... after hydrolosis of raw mdp2p from the wacker and dcm extraction i re-hit the pooled dcm extracts with dcm.... they took a yellow shiney color but interestingly the dcm + dcm layers formed seperate layers... whys that/??
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Tungsten.

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Re: Short Questions Thread
« Reply #1072 on: October 24, 2011, 08:34:08 PM »
Does anyone know if FeCl3 is a strong enough lewis acid for a friedel-crafts alkynation? AlCl3 seems like a pain to make.
-W

akcom

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Re: Short Questions Thread
« Reply #1073 on: October 24, 2011, 09:19:48 PM »
It has to be anhydrous

Tungsten.

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Re: Short Questions Thread
« Reply #1074 on: October 24, 2011, 09:35:01 PM »
I didn't read that FeCl3 had the same issue that AlCl3 did with the hydrate. Well there goes that idea...
-W

lugh

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Re: Short Questions Thread
« Reply #1075 on: October 24, 2011, 10:47:57 PM »
Quote
Well there goes that idea...

Not necessarily, there is a helpful tool called the search engine:

http://127.0.0.1/talk/index.php/topic,289

https://the-collective.ws/forum/index.php?topic=11013

 8)
« Last Edit: October 24, 2011, 10:54:46 PM by lugh »
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Tungsten.

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Re: Short Questions Thread
« Reply #1076 on: October 24, 2011, 11:17:12 PM »
I actually did know about that patent, and that was the plan. Either that or run dried chlorine gas through a heated aluminum tube.

I was just hoping that I could go buy some etchant and bake it. :(

Edit: Why have I never heard of Mn(OAc)3 catalyzed radical alkalynation (halo-ketones scares the shit out of me)? Anyone have a clever synth of anhydr. Mn(OAc)3? Rhodium's synthesis seems very roundabout (and not anhydrous?).

Double edit: Turns out you don't need the anhydrous salt. Why is that?

Also, I really don't want to have to buy a tank of nitrogen in order to do this experiment, is there any way I could use CO2? CO2 seems pretty inert, and I can't imagine that it would effect this reaction much would it?
« Last Edit: October 25, 2011, 08:13:20 PM by Tungsten. »
-W

Vesp

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Re: Short Questions Thread
« Reply #1077 on: October 26, 2011, 04:42:46 AM »


Also, I really don't want to have to buy a tank of nitrogen in order to do this experiment, is there any way I could use CO2? CO2 seems pretty inert, and I can't imagine that it would effect this reaction much would it?

Just jumped in here, so I do not know what you are talking about... but wouldn't something along the lines of propane or butane from a tank work just fine for providing an inert atmosphere? It has a few advantageous off the top...
1. heavier than air
2. Easy to get, control, and regulate flow...
3. Less reactive than CO2, as CO2 can be acidic and who knows, that might be an issue?
And than of course the cons..
1. Might want to clean it with anhydrous NaOH to get rid of any sulfides that could be present?
2. Might want to dry it?
3. It is a fire hazard...
The
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Terror

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Re: Short Questions Thread
« Reply #1078 on: October 26, 2011, 08:04:44 AM »
Has anyone completed the wacker in less than 8 hrs? I read a paper on a 3 hour reaction (small scale) gave it a go but i think my safrole is freezing out of the dcm... the paper confirmed safrole was non existant via gc....
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Tungsten.

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Re: Short Questions Thread
« Reply #1079 on: October 26, 2011, 01:22:16 PM »


Also, I really don't want to have to buy a tank of nitrogen in order to do this experiment, is there any way I could use CO2? CO2 seems pretty inert, and I can't imagine that it would effect this reaction much would it?

Just jumped in here, so I do not know what you are talking about... but wouldn't something along the lines of propane or butane from a tank work just fine for providing an inert atmosphere? It has a few advantageous off the top...
1. heavier than air
2. Easy to get, control, and regulate flow...
3. Less reactive than CO2, as CO2 can be acidic and who knows, that might be an issue?
And than of course the cons..
1. Might want to clean it with anhydrous NaOH to get rid of any sulfides that could be present?
2. Might want to dry it?
3. It is a fire hazard...
The
I didn't even think of propane... Seems less reactive than CO2 (I think?).

Problems that I see with propane: The acetone radical might want to react with propane (although the pka of propane is higher than that of benzene) as apposed to benzene especially because propane is soluble in benzene.

What do you think, would that be an issue (especially during reflux)?
-W