Use algebra.
Baba_McKensey
- Subordinate Wasp
- Posts: 109
Flight
- Larvae
- Posts: 23
Could the mathematical formula be posted?
That would be extremely helpful
That would be extremely helpful
RoidRage
- Dominant Queen
- Posts: 386
C'mon..We're not going to start spoonfeeding high school mathematics
Wizard X
- Lord of the Realms
- Foundress Queen
- Posts: 1,224
Buffered Performic Route....
How does one calculate the amount of H2O2 to use? So instead of using 35% say only 29% is available. Also, is using 29% a good idea or should only 35% be used.
Thanks,
F
The moles of H2O2 required in a balanced equation.
Learn Concentration: Weight/Weight % (AKA Mass fraction)
Conversion of % W/W to Molarity, moles per litre, mol/Lt.
Data required is % W/W and density of the solution.
(% W/W x density) /100 = grams per ml (g/ml)
(grams per ml / formula weight) x 1000 = Molarity, moles per litre, mol/Lt.
Refs:
http://www.iun.edu/~cpanhd/C101webnotes/aqueoussolns/wwpcnt.html
http://pages.towson.edu/ladon/concas.html
http://www.ausetute.com.au/weightpc.html
http://en.wikipedia.org/wiki/Mass_fraction_(chemistry)
Flight
- Larvae
- Posts: 23
Quote
The moles of H2O2 required in a balanced equation.
Learn Concentration: Weight/Weight % (AKA Mass fraction)
Conversion of % W/W to Molarity, moles per litre, mol/Lt.
Data required is % W/W and density of the solution.
(% W/W x density) /100 = grams per ml (g/ml)
(grams per ml / formula weight) x 1000 = Molarity, moles per litre, mol/Lt.
Sorry, not looking to be spoon fed, actually was just needing more of a clarification that the right path was being followed. Thanks for the assistance Wizard X.
Tsjanga
- Larvae
- Posts: 27
If we go from Heli to its oxime form then reduct it to an amine and dehydogenate it would we get easily to some of our favorite mdxx?
pbinteger
- Subordinate Wasp
- Posts: 124
Herro!
I've been reading up on all the variations on the al/hg amalgam. I've noticed that some prefer to wash the excess Hg salts off their aluminum before completing the reaction.
What is the purpose of this?
Thank You
I've been reading up on all the variations on the al/hg amalgam. I've noticed that some prefer to wash the excess Hg salts off their aluminum before completing the reaction.
What is the purpose of this?
Thank You
Scr0t
- Larvae
- Posts: 3
I think it's over concerns of some residual mercury contamination in the product.
https://www.sciencemadness.org/talk/viewthread.php?tid=17479
https://www.sciencemadness.org/talk/viewthread.php?tid=17479
pbinteger
- Subordinate Wasp
- Posts: 124
Hi Scr0t,
This refers to washing the freebase -- which I always do VERY thoroughly followed by a standard acid / base workup.
I was talking about kicking off the amalgam in water, then removing the aluminum and washing it in a strainer to get excess mercuric salts out, then placing it back in MeOH to finish the reaction with MeNH2 or Nitromethane etc...etc..
I was curious what benefit this lends to the reductive amination.
Thanks!
This refers to washing the freebase -- which I always do VERY thoroughly followed by a standard acid / base workup.
I was talking about kicking off the amalgam in water, then removing the aluminum and washing it in a strainer to get excess mercuric salts out, then placing it back in MeOH to finish the reaction with MeNH2 or Nitromethane etc...etc..
I was curious what benefit this lends to the reductive amination.
Thanks!
Scr0t
- Larvae
- Posts: 3
Hello!
I was referring to possible mercuration of the benzene ring by Hg+2 that may be present. Washing the Al is not difficult and gives one peace of mind if you're paranoid about mercury.
I have done Al/Hg reductions of nitrostyrenes with and without washing the Al and have not noticed any difference in yield so I expect it probably wouldn't make any difference, yield wise, with reductive amination.
I was referring to possible mercuration of the benzene ring by Hg+2 that may be present. Washing the Al is not difficult and gives one peace of mind if you're paranoid about mercury.
Quote from: Nicodem
Mercuric(II) salts are strong soft acids which tends to react with soft bases like the Pi-systems of benzene, toluene or other electron rich aromatics via the electrophilic aromatic substitution. It also reacts with the Pi-bonds of alkenes and alkynes as well as other similarly soft bases. The product with benzene or toluene, the corresponding arylmercuric salts, are preferentially partitioned in the organic solvents rather than water.
http://en.wikipedia.org/wiki/Organomercury#Mercuration_of_aromatic_rings
I have done Al/Hg reductions of nitrostyrenes with and without washing the Al and have not noticed any difference in yield so I expect it probably wouldn't make any difference, yield wise, with reductive amination.
pbinteger
- Subordinate Wasp
- Posts: 124
Thanks Scr0t -- that answers my question!
pbinteger
- Subordinate Wasp
- Posts: 124
Does anyone have a ref / link to a write up on
Methyl-3,4-Methylenedioxyhydrocinnamic aldehyde + KMnO4 -> Methyl-3,4-Methylenedioxyphenylpropionic acid + NaN3 + H2SO4 -> MDA
Methyl-3,4-Methylenedioxyhydrocinnamic aldehyde + KMnO4 -> Methyl-3,4-Methylenedioxyphenylpropionic acid + NaN3 + H2SO4 -> MDA
syn
- Larvae
- Posts: 12
Having problems with an oximation.
My numbers are-
2000ml of ethanol
2000ml of water
1000g of aldehyde
1000g of hydroxylamine HCl
580g of sodium carbonate
So the reaction appears to have went a lot better this time. Excess hydroxylamine was used. After basing a bunch of the oxime came out of solution as a powder on the bottom of the flask. Now hears were it gets weird. There is the oxime at the bottom, a layer of water in the middle, and an organic layer at the top. The layer at the top looks just like the oxime I got from the last oximation I did except that was at the bottom. Any help would be appreciated.
My numbers are-
2000ml of ethanol
2000ml of water
1000g of aldehyde
1000g of hydroxylamine HCl
580g of sodium carbonate
So the reaction appears to have went a lot better this time. Excess hydroxylamine was used. After basing a bunch of the oxime came out of solution as a powder on the bottom of the flask. Now hears were it gets weird. There is the oxime at the bottom, a layer of water in the middle, and an organic layer at the top. The layer at the top looks just like the oxime I got from the last oximation I did except that was at the bottom. Any help would be appreciated.
Tsjanga
- Larvae
- Posts: 27
Having problems with an oximation.
My numbers are-
2000ml of ethanol
2000ml of water
1000g of aldehyde
1000g of hydroxylamine HCl
580g of sodium carbonate
So the reaction appears to have went a lot better this time. Excess hydroxylamine was used. After basing a bunch of the oxime came out of solution as a powder on the bottom of the flask. Now hears were it gets weird. There is the oxime at the bottom, a layer of water in the middle, and an organic layer at the top. The layer at the top looks just like the oxime I got from the last oximation I did except that was at the bottom. Any help would be appreciated.
Try to add the hydroxylamine.hcl very very slowly in droplets instead of the whole bunch at once Also stirring the shit out of it?
Is the Sodium Carbonate H2O free?
Does anyone have a ref / link to a write up on
Methyl-3,4-Methylenedioxyhydrocinnamic aldehyde + KMnO4 -> Methyl-3,4-Methylenedioxyphenylpropionic acid + NaN3 + H2SO4 -> MDA
I will send you a PM with some info
Tsjanga
- Larvae
- Posts: 27
Somebody could help me, a friend has found the powdered version of the aldehyde we are talking about here.
Could he just get it and return it to the liquid?
Could he just get it and return it to the liquid?
syn
- Larvae
- Posts: 12
There is no powdered version. The aldehyde is a clear/yellow liquid or it isn't the aldehyde. What do you mean add it in droplets? Hydroxylamine HCl is a powder and adding the solution to your aldehyde in small amounts won't do anything because it has to be the freebase to react. I added all my hydroxylamine HCl in 1 liter of water and added it to the ethanol/aldehyde. Then I added sodium carbonate with stirring over the course of 4 hours a few hundred ml at a time.
The organic layer at the top has now turned slightly brownish. The layer at the bottom is salt so if the oxime did form it's in the organic lay. I'm throwing it on to reflux for a bit. With such a large excess of hydroxylamine present the reaction should have gone. Will run TLC
The organic layer at the top has now turned slightly brownish. The layer at the bottom is salt so if the oxime did form it's in the organic lay. I'm throwing it on to reflux for a bit. With such a large excess of hydroxylamine present the reaction should have gone. Will run TLC
Tsjanga
- Larvae
- Posts: 27
There is no powdered version. The aldehyde is a clear/yellow liquid or it isn't the aldehyde. What do you mean add it in droplets? Hydroxylamine HCl is a powder and adding the solution to your aldehyde in small amounts won't do anything because it has to be the freebase to react. I added all my hydroxylamine HCl in 1 liter of water and added it to the ethanol/aldehyde. Then I added sodium carbonate with stirring over the course of 4 hours a few hundred ml at a time.
The organic layer at the top has now turned slightly brownish. The layer at the bottom is salt so if the oxime did form it's in the organic lay. I'm throwing it on to reflux for a bit. With such a large excess of hydroxylamine present the reaction should have gone. Will run TLC
There is a powdered version, but can we use it that is the question.
Just add the hydroxylamine slowely and then let the Sodium Carbonate drop into the solution don't dump in like 100ml at once but use your funnel or something to let it drip. Here the guy's did it in about 5 hours with droplets and had a great success with dumping a shitload in at once they came up with the same problem you had.
If you want you can send me a PM
antibody2
- Subordinate Wasp
- Posts: 158
teahead - that will depend on the reaction that produced the MDP2P, it might work coming from an O2 wackier, but unlikely to work well coming from a benzo wacker or performic reaction.
Almost every time Ab2 attempted to move onto the next step in a synth without properly purifying things she had poor to horrible results. It really is worth the effort to take the high road. Even if the reaction is partially successful, you will have a difficult time crystallizing your end product, because of all the contaminants that remain.
If you are impatient, go buy a fridge compressor at a used appliance store for $20. They make great disposable vacuums
Almost every time Ab2 attempted to move onto the next step in a synth without properly purifying things she had poor to horrible results. It really is worth the effort to take the high road. Even if the reaction is partially successful, you will have a difficult time crystallizing your end product, because of all the contaminants that remain.
If you are impatient, go buy a fridge compressor at a used appliance store for $20. They make great disposable vacuums
myCH3
- Pupae
- Posts: 77
Quote from: Tsjanga
[quote author=pbinteger link=topic=2962.msg36473#msg36473 date=1367808784
[quote author=pbinteger link=topic=2962.msg36473#msg36473 date=1367808784
Does anyone have a ref / link to a write up on
Methyl-3,4-Methylenedioxyhydrocinnamic aldehyde + KMnO4 -> Methyl-3,4-Methylenedioxyphenylpropionic acid + NaN3 + H2SO4 -> MDA
I will send you a PM with some info
[/quote]
anyway I could get in on that info as well?
Tsathoggua
- Autistic sociopath
- Foundress Queen
- Posts: 662
Can't comment on the peracid rxn, never done it. But a quick look at a bottle of (off the shelf 9%, from the UK, pharmaceutical) H2O2 reveals phosphoric acid, and phenacetin as the other ingredients present.