@ 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.
antibody2
- Subordinate Wasp
- Posts: 158
4studiesonly
- Larvae
- Posts: 28
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
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
lugh
- Global Moderator
- Foundress Queen
- Posts: 876
There's a thread on Science Madness on the chamber process:
http://www.sciencemadness.org/talk/viewthread.php?tid=2824
http://en.wikipedia.org/wiki/Chamber_process
which hasn't been used industrially since the last world war The reaction that produces diethyl ether requires heat:
https://the-collective.ws/forum/index.php?topic=12796.
http://www.sciencemadness.org/talk/viewthread.php?tid=9180
http://www.sciencemadness.org/talk/viewthread.php?tid=771
http://www.sciencemadness.org/talk/viewthread.php?tid=255
http://www.sciencemadness.org/talk/viewthread.php?tid=18719
http://www.erowid.org/archive/rhodium/chemistry/ethyl.ether.html
and many others that can be found with more effort The end results from the effort applied
http://www.sciencemadness.org/talk/viewthread.php?tid=2824
http://en.wikipedia.org/wiki/Chamber_process
which hasn't been used industrially since the last world war The reaction that produces diethyl ether requires heat:
https://the-collective.ws/forum/index.php?topic=12796.
http://www.sciencemadness.org/talk/viewthread.php?tid=9180
http://www.sciencemadness.org/talk/viewthread.php?tid=771
http://www.sciencemadness.org/talk/viewthread.php?tid=255
http://www.sciencemadness.org/talk/viewthread.php?tid=18719
http://www.erowid.org/archive/rhodium/chemistry/ethyl.ether.html
and many others that can be found with more effort The end results from the effort applied
T-cowboy
- Pupae
- Posts: 57
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
- Pupae
- Posts: 84
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
ImA
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
ImA
lugh
- Global Moderator
- Foundress Queen
- Posts: 876
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 The end results from the effort applied
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 The end results from the effort applied
EMTWC
- Larvae
- Posts: 28
Hg/Al amalgam ran too hot. got up to about 70 in the ice bath.
product scorched?
product scorched?
RoidRage
- Dominant Queen
- Posts: 386
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
- Larvae
- Posts: 11
Can anyone point me in the right direction of a Hydroxlamine to Ketamine synthesis. I cannot find any info regarding it.
Thanks.
Thanks.
dream0n
- Subordinate Wasp
- Posts: 204
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 -- But you would want to spell it right first.
d1ssonance
- Larvae
- Posts: 11
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 -- 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
nigluhS
- Pupae
- Posts: 81
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"?
ImAMANGUYS
- Pupae
- Posts: 84
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
ImA
myhero
- Pupae
- Posts: 80
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?
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
- Larvae
- Posts: 33
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.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.
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?
4studiesonly
- Larvae
- Posts: 28
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...
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...
myhero
- Pupae
- Posts: 80
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
- I can ride my bike with no handlebars
- Pupae
- Posts: 61
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
- Larvae
- Posts: 28
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?
Trying to boil off IPA, brightstar synth says 35 under vacuum.
is product coming over with the IPA at 55 w/o vacuum?
RoidRage
- Dominant Queen
- Posts: 386
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...