Author Topic: Short Question Thread 2.0  (Read 5709 times)

antibody2

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Re: Short Question Thread 2.0
« Reply #260 on: January 11, 2013, 12:48:13 AM »
@ pbinteger - not if your vacuum is strong enough. Although it isn't usually necessary to purify the intermediate, just proceed directly to the hydrolysis step.

4studiesonly

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Re: Short Question Thread 2.0
« Reply #261 on: January 13, 2013, 04:53:33 PM »
So...
About my post above.
I have now looked more into this but i cant work out if this works or rather where it fails.
If things were a bit different i would just try it out, but i cant 4 now.

I searched some more and found this: sciencemadness.org/talk/viewthread.php?tid=1426
And already in the 6:th post the creator states " Ah I see your point" to those in doubt, but hey i do not see his point.
The doubt here being that NaHSO4 is not soluble in alcohol(well, not only that), yes ok
But that is not the idea either, the idea is that it decomposes as stated in post above.
There is of course something wrong here, for one thing, it is impossible to go absolutely anhydrous here and there would be some H2O present. I guess this will fuck up things even outside my troubled mind....

They mention that any water present will dissolve any Na2SO4 formed, yes i guess so and that will make me cry why?
That the alcohol will distill/evaporate before the water i get but would that be a problem, that is in my favor is it not?

I also now read about dehydration of ethanol at ucc.ie/academic/chem/dolchem/html/comp/ethanol.html and that yielded me
"When ethanol is mixed with concentrated sulphuric acid with the acid in excess and heated to 170 degC, ethylene is formed."
But i wont heat the mixture, so? And then from same source.
"When ethanol is mixed with concentrated sulphuric acid with the alcohol in excess and heated to 140 degC, diethyl ether distills over".
But again i wont heat the mixture so?

It all comes down to this (i now think, learning as i am writing this), is the production of diethyl ether gonna happen at roomtemperature? What if one worked in lets say a freezer? I am grasping for hope here, but i guess there are none....
Is the patient dead yet?


Edit:

2 NaHsO4 + C2H5OH ---->
H2SO4 + Na2SO4  + C2H5OH

----->

Both Na2SO4 and C2H5OH then reacts with the formed H2SO4 in 2 simultaneous
reactions.

------->

1. Na2SO4  + H2SO4 ------> 2 NaHSO4  which then reacts with excess of C2H5OH and so on...
2. C2H5OH + H2SO4 -------> (in room temperature) C2H6O4S (ethyl sulfate) + H2O will form but this is a exothermic reaction and at 140 degrees(does it go to this temp by it self or will heat need to be added?) ----->
according to ucc.ie/academic/chem/dolchem/html/comp/ethanol.html
Ethanol in excess is mixed with sulfuric acid diethyl ether is formed like this:
                                         H2SO4
2 C2H5OH      ==>     C2H5OC2H5     +      H2O
                                          140 deg
Now i do not get where the S has gone to?
And the same question appears if the temp instead jumps up to 170 degrees, cause then:
H2SO4
C2H5OH         ==>     C2H4 + H2O
170 degC

 ==>     C2H5OC2H5

Either way i am now pretty sure this is the definition of a dead end, but i still would like to know the answers to my questions and reflections
« Last Edit: January 13, 2013, 07:01:49 PM by 4studiesonly »
Bis zum bitteren ende

lugh

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Re: Short Question Thread 2.0
« Reply #262 on: January 14, 2013, 12:27:47 AM »
Chemistry is our Covalent Bond

T-cowboy

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Re: Short Question Thread 2.0
« Reply #263 on: January 15, 2013, 12:05:09 PM »
I read in A Laboratory History of Narcotics, Vol. 1 Amphetamines and Derivatives there is some sort of ritter reaction but not really. where safrole reacts with cyanide (no refs given) to give mda. i know that the ritter does not like the methylene brige. but has anyone got a ref for this or info?

ImAMANGUYS

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Re: Short Question Thread 2.0
« Reply #264 on: January 17, 2013, 07:47:22 PM »
How can one tell what kind of vacuum a pump will pull?

I've used the search engine and found that more stages make for a better vacuum. If one were to only buy a single stage, what kind of CFM would be needed to pull ~29''hg.

I'm currently viewing amazon and ebay and deciding which to buy.

Thought some of you might have some experience :P

ImA

lugh

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Re: Short Question Thread 2.0
« Reply #265 on: January 17, 2013, 09:24:08 PM »
You apparently didn't use the search engine very well:

http://127.0.0.1/talk/index.php/topic,2547.msg25798.html#msg25798

or you would have downloaded that old ebook  ;) There's also the links provided in:

http://127.0.0.1/talk/index.php/topic,2962.msg33324.html#msg33324

which is from this very thread ::) There are other posts useful to you here and at other web sites from other knowledgeable members as well as this one   :P  The end results from the effort applied  8)   
Chemistry is our Covalent Bond

EMTWC

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Re: Short Question Thread 2.0
« Reply #266 on: January 22, 2013, 06:08:57 PM »
Hg/Al amalgam ran too hot. got up to about 70 in the ice bath.

product scorched?
roll some bones and catch a fire

RoidRage

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Re: Short Question Thread 2.0
« Reply #267 on: January 22, 2013, 08:29:44 PM »
Hg/Al amalgam ran too hot. got up to about 70 in the ice bath.

product scorched?

Product certainly won't decompose much under a temperature of 150 celsius degrees.

d1ssonance

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Re: Short Question Thread 2.0
« Reply #268 on: January 23, 2013, 05:36:35 AM »
Can anyone point me in the right direction of a Hydroxlamine to Ketamine synthesis. I cannot find any info regarding it.


Thanks.

dream0n

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Re: Short Question Thread 2.0
« Reply #269 on: January 23, 2013, 06:08:02 AM »
There was one over at http://www.sciencemadness.org/talk/viewthread.php?tid=6531 , but it isn't hydroxlamine or hydroxylamine, it is an -imine  Even spouted off the basics at zotlek- should be able to find something, even if not in this forum :D  -- But you would want to spell it right first. 
off to bigger and better things - don't worry I will visit from time to time

d1ssonance

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Re: Short Question Thread 2.0
« Reply #270 on: January 23, 2013, 07:13:11 AM »
There was one over at http://www.sciencemadness.org/talk/viewthread.php?tid=6531 , but it isn't hydroxlamine or hydroxylamine, it is an -imine  Even spouted off the basics at zotlek- should be able to find something, even if not in this forum :D  -- But you would want to spell it right first.

Yeah, I saw the SM hydroxyimine synth.

What I'm looking for is info regarding hydroxylamine.

Reason why i'm curious is it's sale is now restricted in China, and it's highly sought after in NL.

Do a quick google search and you will see that several reputable sources name Hydroxylamine as the immediate precursor of ketamine.

It could just be that the sources were wrong, it's just that one of them was an article cited by the WHO. lol


« Last Edit: January 23, 2013, 07:23:37 AM by d1ssonance »

nigluhS

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Re: Short Question Thread 2.0
« Reply #271 on: January 23, 2013, 12:14:53 PM »
Hg/Al amalgam ran too hot. got up to about 70 in the ice bath.

product scorched?

Product certainly won't decompose much under a temperature of 150 celsius degrees.

thanks RR...what does brightstar say to "DEFINITELY keep it under 60 degrees"?
when the wasps and the bumblebees have a party, nobody comes that can't buzz...

ImAMANGUYS

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Re: Short Question Thread 2.0
« Reply #272 on: January 23, 2013, 03:40:23 PM »
To minimilize size reactions as well as keeping the reaction under control... (I believe!) i think i recall something about IPA resulting in more than a few runaway amalgams... I may be wrong but i believe this is why methanol is now the solvent of choice (low bp which controls side reactions and keeps temps somewhat controlled)

ImA

myhero

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Re: Short Question Thread 2.0
« Reply #273 on: January 24, 2013, 10:01:24 AM »
I was recently isomerizing 890ml of a certain oil fraction a la OcoteaCymbarum (20hours @150°C with no CaO). I Used around 2.5% weight (23g) of 85% KOH. After isomerization completed (20 hours later), I distilled the resulting compound over a range of 10°C, around 20°C higher than the original non isomerized compound. I recovered a 98% yield, ending up with mostly a dry 2L boiling flask.

When I washed the flask afterwards I had no issue removing the KOH but, like it happened before with another flask the glass seemed etched, corroded where the KOH deposited. The flask is still usable I guess althouh I am a bit sorry for the damage ...

Has anyone had this issue before?

Gypsy

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Re: Short Question Thread 2.0
« Reply #274 on: January 24, 2013, 11:34:05 AM »
I was recently isomerizing 890ml of a certain oil fraction a la OcoteaCymbarum (20hours @150°C with no CaO). I Used around 2.5% weight (23g) of 85% KOH. After isomerization completed (20 hours later), I distilled the resulting compound over a range of 10°C, around 20°C higher than the original non isomerized compound. I recovered a 98% yield, ending up with mostly a dry 2L boiling flask.

When I washed the flask afterwards I had no issue removing the KOH but, like it happened before with another flask the glass seemed etched, corroded where the KOH deposited. The flask is still usable I guess althouh I am a bit sorry for the damage ...

Has anyone had this issue before?
yeah. been careless now and again dissolving even naoh. etches in. gotta watch out and keep your ground glass neck joints clean. have become rather paranoid about that.

4studiesonly

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Re: Short Question Thread 2.0
« Reply #275 on: January 24, 2013, 12:16:23 PM »
I miss a way to get all the subjects started by a user in front of me.
When i am on a users profile there is the "show posts" link to click on but it would be great if there was a "show started subjects/threads" button.
I have tried through the search function and write a users handle and checked the topics only box but then there is the issue with the lacking of "something to search for".

Am i missing something or is this not possible, cause it would be nice since some of you have contributed with a lot 4 someone like me to read...
Bis zum bitteren ende

myhero

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Re: Short Question Thread 2.0
« Reply #276 on: January 24, 2013, 12:50:59 PM »
Quote
I was recently isomerizing 890ml of a certain oil fraction a la OcoteaCymbarum (20hours @150°C with no CaO). I Used around 2.5% weight (23g) of 85% KOH. After isomerization completed (20 hours later), I distilled the resulting compound over a range of 10°C, around 20°C higher than the original non isomerized compound. I recovered a 98% yield, ending up with mostly a dry 2L boiling flask.

When I washed the flask afterwards I had no issue removing the KOH but, like it happened before with another flask the glass seemed etched, corroded where the KOH deposited. The flask is still usable I guess althouh I am a bit sorry for the damage ...

Has anyone had this issue before?

I was talking about the flask, not so much the joints.

I'll see if I can post a picture anytime soon

Whale

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Re: Short Question Thread 2.0
« Reply #277 on: January 24, 2013, 01:59:53 PM »
I miss a way to get all the subjects started by a user in front of me.
When i am on a users profile there is the "show posts" link to click on but it would be great if there was a "show started subjects/threads" button.
I have tried through the search function and write a users handle and checked the topics only box but then there is the issue with the lacking of "something to search for".

Am i missing something or is this not possible, cause it would be nice since some of you have contributed with a lot 4 someone like me to read...

If you go to their profile and click see thier posts at the top there will be like posts topics and some other shit. Click on topic and itll show all of thier threads

EMTWC

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Re: Short Question Thread 2.0
« Reply #278 on: January 24, 2013, 07:48:30 PM »
on the lowest setting, the heating mantle gets up to 55 and that's WITHOUT vacuum.
Trying to boil off IPA, brightstar synth says 35 under vacuum.

is product coming over with the IPA at 55 w/o vacuum?
roll some bones and catch a fire

RoidRage

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Re: Short Question Thread 2.0
« Reply #279 on: January 25, 2013, 07:13:02 PM »

thanks RR...what does brightstar say to "DEFINITELY keep it under 60 degrees"?

ImAMANGUYS named a few viable points.

Important thing to remember though, is that while Methyl Man/ Bright Star's write-ups works and are perfect for beginners, they're far from being optimized and contains some chemistry non-sense  ;). Just to let you knows,I never ran an amalgam under 65 degrees. Runaways reactions can occurs at any temperature. I remember reading something about amalgams being an explosion hazard over a certain temperature but I don't remember the source + I don't know how it can happens...