I can bring NaBH4 dissolved in methanol
- Thread starter bitcoinup2020
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MDP2P needs to be reacted with methylamine to form an imine which can then be reduced with NaBH4 (even better is Na triacetoxy borohydride)
What proportion should I use for triacetoxy borohydride?
And what method should be used to reduce mdp2p to mdma?
Thank you very much for your help.
And what method should be used to reduce mdp2p to mdma?
Thank you very much for your help.
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- By LazZzZz
Sodium triacetoxyborohydride is sodium borohydride reacted with glacial acetic acid, while yes it is better as a selective reducing agent, what herr as forgot to mention was that sodium triaxetoxyborohydride will hydrolise easily when presented with water, so any aqueous methylamine will react, I either reccomend scooping in the borohydride with a spoon in small portions to the reaction mix with heavy stiring and in a cooled bath, or instead using sodium cyanoborohydride with methylamine HCl, using sodium cyanoborohydride will give you yeilds of 95% however the write up will cause HCN to be produced so there is that causion
can i use sodium cyanoborohydride at the same rate as sodium borohydride?
For example, 1000 g of mdp2p uses 100g of sodium borohydride.
Can use mdp2p 1000 g use sodium cyanoborohydride 100g?
And can I use the method with a spoon in small portions to the reaction mix with heavy stiring and in a cooled bath?
Thank you very much for the answer and help.
For example, 1000 g of mdp2p uses 100g of sodium borohydride.
Can use mdp2p 1000 g use sodium cyanoborohydride 100g?
And can I use the method with a spoon in small portions to the reaction mix with heavy stiring and in a cooled bath?
Thank you very much for the answer and help.
- By OrgUnikum
You can use it, it is actually very well suited for the task but you face the problem of cyanide formation on contact with acids and without a VERY good post-reaction workup there will be always at least traces of cyanide in the final product, what usually throws customers into hysteric fits should they find Cyanide listed in the test even if its in completely insignificant amounts.
It is also very expensive whilst STAB can be made by oneself just for the cost of the acetic acid. Of course one needs much much more from Cyano or STAB then from NaBH4 itself, STAB and Cyano effectivly only donate less then one hydrogen to the reduction, NaBH4 provides theoretically four - practically more like two and a half.
It is also very expensive whilst STAB can be made by oneself just for the cost of the acetic acid. Of course one needs much much more from Cyano or STAB then from NaBH4 itself, STAB and Cyano effectivly only donate less then one hydrogen to the reduction, NaBH4 provides theoretically four - practically more like two and a half.
- By LazZzZz
Again the issue comes from STABs inability to react with water, and sodium cyanoborohydride costs maybe 80 dollars a kg from ali or other reselling websites, and as long as you perform a distilation of the freebase amine under vaccume, you can eliminate any HCN by reacting the extracted free base with conc sodium hydroxide
"Yeah bro just perform a vacuum distillation, no big deal" he said to the user that doesn't grasp molarity.
- By OrgUnikum
NaBH4 itself does virtually not react with water and methanol as long the temperature is low enough <15 °C and the environment is strongly alkaline. Under this conditions yields of > 90% of theory can be achieved for MDMA.
Stating the obvious: "Strongly alkaline" aka very basic is easy with a good amount of NaOH or sodium methoxide. Of course water content should be kept as low as possible. But this way ~250 g NaBH4 or less are enough to process 1 kg of MDP2P and this means less reaction volume and easier workup.
Stating the obvious: "Strongly alkaline" aka very basic is easy with a good amount of NaOH or sodium methoxide. Of course water content should be kept as low as possible. But this way ~250 g NaBH4 or less are enough to process 1 kg of MDP2P and this means less reaction volume and easier workup.
How much water should I mix for 250 g NaBH4?
and how much NaOH should be added
Should distilled water be at 15 degrees or not?
Thank you very much for your help.
and how much NaOH should be added
Should distilled water be at 15 degrees or not?
Thank you very much for your help.
Sodium borohydride will react with water to release hydrogen even with sodium hydroxide acting as a spectator ion, due to an imine formation being reversible due to water then this is going to be a less than efficient method as methylamine HCl will react with the borohydride in a simple acid base reaction, even if you were to pump anhydrous methylamine into methanol and used that, you'd still only achieve 65-70% due to temperature increases on a molecular scale that lead to things like dimerisarion. Sodium cyanoborohydride is still the best for reduction of imines as methylamine HCl is usable and it means everything can just be dissolved into 1 big tub and stirred for 2-3 days. Along as you do the quenching outside then you'll be fine, just don't huff the gas
Does anyone have any papers on the Sodium cyanoborohydride reduction ? Or are there any posts?
Is the imine formed with ketone and MeAm HCL ? What is the reaction solvent used, is a water scavenger used
Is the imine formed with ketone and MeAm HCL ? What is the reaction solvent used, is a water scavenger used
- By LazZzZz
Its not too difficult, i have a rough explanation
First step is calculation of mols, for every mol of ketone that you use, youll use a 50% excess of sodium cyanoborohydride and a 5X molar excesss when adding the methylamine HCL, this may seem like a lot but it is neccicary. if you use 1 mol of ketone youll want 1.5 mols of cyano and 5 mols of MeNH3Cl and be sure to dissolve everything in plenty of methanol. No water scavengers are used as the reaction will take place over a number of days leading to a nearly quantitative yeild. Once the reaction has completed, the excsess cyanoborohydride are destroyed with either HCl or acetic acid and all of the methanol will be removed (preferably in a rotovap). Once all the methanol has evaporated youll need to redisolve the cake into water and slowly add a concentrated sodium hydroxide while keeping temperatures down. Finally add a non polar solvent like xylene or toluene and perform a water wash, sodium bicarbonate wash and finally a sodium chloride wash and separate the organic layers. Bubble HCl gas through the solvent with the freebased amine and place in buchner funnel and washed with ice cold acetone. To recrystalise then bring a 50%50% IPA:H2O solution a boil and add 1 gram of amine per 3ml and leave to evaporate over a couple of days, enjoy
First step is calculation of mols, for every mol of ketone that you use, youll use a 50% excess of sodium cyanoborohydride and a 5X molar excesss when adding the methylamine HCL, this may seem like a lot but it is neccicary. if you use 1 mol of ketone youll want 1.5 mols of cyano and 5 mols of MeNH3Cl and be sure to dissolve everything in plenty of methanol. No water scavengers are used as the reaction will take place over a number of days leading to a nearly quantitative yeild. Once the reaction has completed, the excsess cyanoborohydride are destroyed with either HCl or acetic acid and all of the methanol will be removed (preferably in a rotovap). Once all the methanol has evaporated youll need to redisolve the cake into water and slowly add a concentrated sodium hydroxide while keeping temperatures down. Finally add a non polar solvent like xylene or toluene and perform a water wash, sodium bicarbonate wash and finally a sodium chloride wash and separate the organic layers. Bubble HCl gas through the solvent with the freebased amine and place in buchner funnel and washed with ice cold acetone. To recrystalise then bring a 50%50% IPA:H2O solution a boil and add 1 gram of amine per 3ml and leave to evaporate over a couple of days, enjoy