Aluminium amalgam (Al/Hg) Summary
no. it will doesn't work... "why ?"
cause what is the element used in this reaction, is the aluminum !
the works of the mercury it's to create a amalgam. and by this way take off the lay of "alumine (the natural oxidation from the air on aluminum")
-for others ways to a amine is :
*LiAlH4 (Lithium aluminum hydride), less toxic, pretty unstable/ hard to find.... easy if you are a professional cause is one of the easiest reduction.
*or the couple Zn/Ni but i have tried this method
if someone else has other information should be nice to share it here as well.
cause what is the element used in this reaction, is the aluminum !
the works of the mercury it's to create a amalgam. and by this way take off the lay of "alumine (the natural oxidation from the air on aluminum")
-for others ways to a amine is :
*LiAlH4 (Lithium aluminum hydride), less toxic, pretty unstable/ hard to find.... easy if you are a professional cause is one of the easiest reduction.
*or the couple Zn/Ni but i have tried this method
if someone else has other information should be nice to share it here as well.
- By waltjr5858
Actually the lithium aluminum hydride is absolutely not the easiest reduction. I have hundreds of grams of that stuff and it's very easy to buy. I followed protocol exact same Reaction Time same exact amounts and the product is at best a 30% yield and it is all kinds of mixed with side products... yes it will reduce the double bond and the Nitro group but it leaves behind a ton of oxime... hydroxylamine and whatever else. I think the best reduction is the aluminum amalgam but that reaction is extremely finicky and if you can't get the amalgam perfect it won't go. Then we have the copper and borohydride which is great but I found that the laurelhydride has to be pretty damn fresh.
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- By waltjr5858
Borohydride.... I have definitely wasted hundreds of grams of p2np on all different type of reactions. Another fairly clean way which is posted on this site is using zinc but the directions as they are posted do not work and I believe the poster that put them up said he just found them on the Internet and was going to give them a try. Using tin 2 chloride well absolutely give high yields of ketoxime and absolutely no acid needs to be added just the tin and the p2np. Allow that to run for maybe an hour or so and the exothermic reaction will come back to room temperature and you can kind of use their instructions for extraction for the next step. The Next Step requires an adjustment from what they put otherwise yes the oxime will go to amine but the double bond will remain. Use zinc and glacial acetic acid but take it up to reflux for 4 hours and that will saturate the double bond. A lot of write-ups say it will tolerate the double bond but they are also only doing 5 minute reactions to reduce the oxime to Amine and leaving the double bond. Another poster on the reaction on here somewhere used glacial acetic acid and a little bit of HCL when he did it and was successful. I tried it both ways with a dash of HCL on one maybe 10 mL to the whole reaction and just with GAA. Both fully successful. But more work than the aluminum amalgam. Although that damn amalgam can be tough to get right
In your place I would simply test with a small load if you have gallium available and report the result here.
Gallium forms an amalgam with aluminum just like mercury and produces hydrogen, but there are also some differences at the electron level that make mercury impossible to replace with gallium completly.
Gallium forms an amalgam with aluminum just like mercury and produces hydrogen, but there are also some differences at the electron level that make mercury impossible to replace with gallium completly.
- By waltjr5858
Exactly... this reaction is an electron swap between the aluminum and p2np. The hydrogen is actually bad for the reaction. But if the amalgam is right it will go.
Here also a reduction without mercury, I find very interesting and reads easy, I will also try sometime.
I see no reason why gallium amalgamation shouldn't work. But to produce the al/ga amalgamation beforehand, I think you need a gallium salt. Otehrwaise maybe just try with a bit of gallium and alufoil in a rb flask, swirl it around until you can see them reacting. Then add P2NP and see if it reduces?
You could probably produce gallium chloride by dissolving gallium in concentrated HCl, then add that to aluminium foil. If you don't want to loose P2NP, you could always try to just add the amalgamated foil to water. If it produces bubbles, that's hydrogen gas from the reduction of H2O by the exposed aluminum.
I don’t know if you are aware but gallium forms amalgams with metals, including Al.Everything you said about Hg in the first paragraph can be applied to gallium.Please correct me if I’m wrong, anyone.
I read about liah, I don’t wanna work with it at the moment, too dangerous in my setting, And about Zn/Ni I dont know about at all, is there any info here? Thanks.
I read about liah, I don’t wanna work with it at the moment, too dangerous in my setting, And about Zn/Ni I dont know about at all, is there any info here? Thanks.
question: im following the rinse x 3 method, to eliminate as much mercury as possible, but iw we choose for example IPA as the solvent, the old rhodium/osmium synth , (in IPA or methanol) they dont rinse, and i suppose they belive all the mercury salts will be out of the mix when alkali/acid steps are done.... so... what you guys think about it?
the rinses when water is used could affect the final yield?
they say the yield is 90% of the mdp2p , which is a lot more of my yields...could be that the reason?
im doing microscale , but it shouldnt be the problem...
the rinses when water is used could affect the final yield?
they say the yield is 90% of the mdp2p , which is a lot more of my yields...could be that the reason?
im doing microscale , but it shouldnt be the problem...
ive not closed in last synths, but after reading some interesting synth routes, some people put it at refluxoin to avoid methylamine loss... that sounds very logic, this could be the reason for lowering of final yields, less methylamine in the amalgam. im planning to use a single neck and put a condenser to reflux..... what you guys thinks about it?
as for my amalgamations, i just wait till bubbles+grey dots appears and rapidly discard water and rinse.... 3 times! .. my amalgam delayed more than 6 hours and final yield not as expected...well, i use thick AL foil in squares (my mistake) but was difficult to reach always 60º celsius and never got 100% AL "melted" , so i will try what Diogenes said, just discard the most water possible in 10 seconds and add the solvents and goods...then later in alkali acid purifications should go out the mercury..... im right?
the low temp, and delay on amalgam saying that im not doing all right..... im sure the rinses are the problem.
as for my amalgamations, i just wait till bubbles+grey dots appears and rapidly discard water and rinse.... 3 times! .. my amalgam delayed more than 6 hours and final yield not as expected...well, i use thick AL foil in squares (my mistake) but was difficult to reach always 60º celsius and never got 100% AL "melted" , so i will try what Diogenes said, just discard the most water possible in 10 seconds and add the solvents and goods...then later in alkali acid purifications should go out the mercury..... im right?
the low temp, and delay on amalgam saying that im not doing all right..... im sure the rinses are the problem.
What is it? Reflux condenser???
It is need to use in amph synthesis (look at manual topic!)
No, you should clean up your amalgam from acid (HNO3 is produced after Al+Hg(NO3)2 reaction).
Hg salt isn't dissolve in these solvents.
It is need to use in amph synthesis (look at manual topic!)
No, you should clean up your amalgam from acid (HNO3 is produced after Al+Hg(NO3)2 reaction).
Hg salt isn't dissolve in these solvents.
- By diogenes
Hi Patton, I meant the Hg salt will remain in the discarded water phase, it`s solubility is very low in IPA. Rinsing is always recommended of course.
- By diogenes
Thank you Patton, you have finally confirmed my theroetical speculations here: http://bbzzzsvqcrqtki6umym6itiixfhn...hesis-from-p2np-via-al-hg-video.196/post-5921
This is real science and is extremely reassuring. My currilent post was only to add my experimeting that using a thicker foil, wasing only once and rinsing as quick as possible, it can still work perfectlty.
This is real science and is extremely reassuring. My currilent post was only to add my experimeting that using a thicker foil, wasing only once and rinsing as quick as possible, it can still work perfectlty.
man, to be honest , you should have a bit more of patience, and maybe dont think the people are stupid just because are asking something thah you know easily....
anyway, you replied something very different in this thread about when start to add the ketone and methylamine after amalgam started, ive correctly asked about the best moment to add those, and as diogenes said for example, and you were agreed, the best moment is when the first 3 signs appears instead to wait too much...
thats what im asking for, i know how to do amphetamines.
i can understand those questions are boring for you, then i would recommend you to not reply to it.
i know deeply a lot of things in a lot of fields and if i really want to help, ill do kindly , because someone have the same doubt you had time ago.
dont take as an ofense, just saying.
as for the non english people trying to talk, be patient sir, there are much more people in the world talking spanish than english, and when a tourist or someone come to my country and at least try to talk spanish im always happy , kind and patient.
the other day i had to reformulate a question just because you think we all have to speak perfectly english..and every single person that readed it , for sure understood it.
anyway, you replied something very different in this thread about when start to add the ketone and methylamine after amalgam started, ive correctly asked about the best moment to add those, and as diogenes said for example, and you were agreed, the best moment is when the first 3 signs appears instead to wait too much...
thats what im asking for, i know how to do amphetamines.
i can understand those questions are boring for you, then i would recommend you to not reply to it.
i know deeply a lot of things in a lot of fields and if i really want to help, ill do kindly , because someone have the same doubt you had time ago.
dont take as an ofense, just saying.
as for the non english people trying to talk, be patient sir, there are much more people in the world talking spanish than english, and when a tourist or someone come to my country and at least try to talk spanish im always happy , kind and patient.
the other day i had to reformulate a question just because you think we all have to speak perfectly english..and every single person that readed it , for sure understood it.
as well , im clearly asked about the synth, methos can be found in rhodium etc... they dont rinse the amalgam, as well because they dont use water, they dilute in IPA or methanol... so... if there is any culprit, are them! haha
those guys knows what they are doing, i suppose they eliminate mercury in alkali/acid steps. you say that mercury doesnt dissolve on those solvents, but, they just dont get rid of mercury? never? thats my original question
those guys knows what they are doing, i suppose they eliminate mercury in alkali/acid steps. you say that mercury doesnt dissolve on those solvents, but, they just dont get rid of mercury? never? thats my original question
OH man.... why i readed this..... now im becoming crazy to found the appropriate one.... almost no one aluminum can be found with purity data.... found only one, but will delay 4 days or so haha... been reading about purity of comertial grade al foil ...and found some guys making a 6 samples study, and they found 5 of 6 have close to 99% ....do you think the commercial grade al is bad stuff? im using a 30 micrones thuckness foil used for put and smoke sishas etc.... not i dont know if im having a loss of yield due to poor quality..
I'm extremely patient, man. Every day I answer to same questions. I'm a little bit confused when person don't try to write correctly question and than offend me that i'm not patient, lol. I can't read your minds... try to read what did you write before posting please.
You are good person but here not a touristic place, here is chemical forum. I try to help you but I can't understand what do you want to say. It is a little bit harder than say of direction in a street.
Mercury isn't bounded (connected) with amph free base. When you make extraction from amalgam solution, Mercury remain in water (which than be discarded).
that bad english crossed the globe and never had problems...maybe i talk weird, but enough to understand, my english is auto learned, at least i try, but Sir, ill use the translator for you haha...kidding, i suppose you are bored to reply the same things day by day.