Meow Meow "Voss" synthesis

[WillD]

Today we will analyze the complete synthesis of meow meow in a glass "Voss" water bottle. As you can see in the photo, we will also need a measuring jug and a syringe. Let's get started!

Measured 100mL of 4-methylpropiophenone and added it to the "Voss" bottle.

Measured 76mL of aq.HBr48% and added it to the "Voss" bottle.

Measure 35% hydrogen peroxide with a syringe (we will need ~29mL in total) and add it drop by drop to our mixture. In the process of addition, red bromine appears.

After adding 1-3 drops, shake the "Voss" bottle until the red color disappears. We repeat this until all the peroxide has been added and the mixture becomes discolored when shaking the bottle.

After adding the peroxide, leave the mixture to crystallize. The top layer will become solid, but sediment may form if you shake during crystallization.

Add 400mL of ethyl acetate, shake until the solid crystallized sediment is completely dissolved and separate the remaining water.

Add 200ml 40% aq. methylamine and shake the "Voss" bottle vigorously for 20 minutes. The mixture will heat up and change color. Do not leave the lid closed for a long time, the bottle may explode.

After 20 minutes, let the mixture stand until the layers separate and separate the top layer from the water.

Add approximately 35-40mL of 48% aq. HBr, shaking after 1-3 drops. We get the lower water layer with crystallized meow meow, which can now be filtered.

But we will do it differently and recrystallize this sediment from water. We add pure water in portions and shake until all the powder is dissolved. Then we separate it into a glass flat Pyrex container and put it in the fridge. This method will allow the impurities to remain in the ethyl acetate layer, which we discard.

After 12 hours in the fridge we have obtained a small needle crystal but throughout the entire volume of the mother liquor. We can filter this.

But if you don't have filtration equipment, this can be problematic. To get a larger crystal we have to use extra water if you use a fridge. Or about the same amount of water if you crystallize at room temperature. This will take longer, coming soon in a new part...

Drink water, be happy!

 

[animeboro]

Hello sir how much finish product you get this way?
How looks like finish product ?
Why u dont use freezer to get finish product ??
Why you wash freebase only one time no 3time water and water and baking soda ?
Why acid hbr ??

 

[WillD]

We will write the quantity after, in large crystals. But based on the used amount of acid there about 100 g of product in the form of salt. Expect a photo of a recrystallized product, this part will be supplemented in the same simple format as synthesis. For crystallization, a refrigerator (~+4*C) is used, you will soon see why and I will give explanations. Washing with water is desirable, we used it but did not write here. Soda was not used for some reason to avoid hydrolysis of ethyl acetate. It will be more difficult to separate. HBr was available, this was already used in the first stage, so we decided to use HBr in the last stage. In addition, crystals are better, and as you see in the last photo, crystallizes even in water almost instantly.

 

[WillD]

In addition, acidification with HBr possible without the use of litmus strips, everything is easily controlled visually when the acids become enough. This can be seen when adding drops, how it reacts. Do you get a powder at once or a red cloud. Then you need to stop adding acid.

 

[animeboro]

so in this case, when HBR is used, there is no need to explain it to get mmc hcl, but if we use HBR, mmc hbr crystal is produced, am I right? you say that 100% of mmc efficiency is maintained with 4methylenopropiophenone, right? and what is the efficiency from 4methylenopropiophenone to 2bromo4methylenopropiophenone, more than 100%? if the efficiency from 4methylenopropiophenone to 2b4m is more than 100%, then the mmc efficiency cannot be 100% efficiency, am I right?

 

[WillD]

Yes, you right. We get hydrobromide. Efficiency is more than 90%. Approximately 140g for BK.

 

[animeboro]

if you get 150g or more of 2b4m from 4methylenopropiophenone, then you need to use more ethyl acetate, why is it that they use a solvent, then the efficiency is lower it should always be 100g 2b4m 500ml ethyl acetate I already tested it once, I used 300ml ethyl acetate and the efficiency was much lower.
if you get 150g or more of 2b4m from 4methylenopropiophenone, then you need to use more ethyl acetate, why is it that they use a solvent, then the efficiency is lower it should always be 100g 2b4m 500ml ethyl acetate I tested it once, I used 300ml ethyl acetate and the efficiency was much lower, correct me if I'm wrong. The hbr method to obtain 2b4m is the best, although expensive, in some countries hbr is as cheap as hcl and in some it is 10x more expensive. The same applies to perhydrol - it is almost impossible to obtain because it is a substance used to produce bombs. but a concentration of 12% is legal, so it can also be emphasized that you can use 12% perhydrol, but you need to use much more of it

 

[animeboro]

then the efficiency is +/-70% mmc hbr with 100ml of 4methylenopropiophenone, to increase the efficiency you need to use 1 more ethyl acetate then synthesis i.e 750ml ethyl acetate another thing, we shake it not for 20 minutes, but for 35 minutes +/- and set aside for 1.5 hours, because the reaction ends when the bottle starts to cool itself, so we know that the reaction is over. and we obtain and set aside so that all 2b4m has reacted with methylamine. better synthesis is dcm+nmp, then the efficiency is much higher

 

[WillD]

There is a little secret for the amount of ethyl acetate. You can cool the mixture immediately after 20 minutes of reaction under running cold water directly in the "Voss" bottle. And it is advisable for you to do the same before acidification and is possible in the process of acidification. Then the amount of ethyl acetate, which we wrote, will be enough. All problems due to hydrolysis during overheating.

 

[WillD]

I do not recommend leaving this synthesis for extra time. For small quantities, this is not so noticeable, but if you make a large scale, it will be significant. The synthesis with NMP also has a place to be, but requires large amounts. NMP is an expensive solvent, and we are looking for simpler and more cheap routes.

 

[dnBQByvHb8Zkawbjpx]

Legend!

Now, where do I get HBr in required quantities and concentration in the EU as a casual consumer? Is making it at home the only way? Similarly, how do I get or I purify hydrogen peroxide to 35 % when all I can get is max 10 %?

 

[WillD]

Not sure that 10% will work. We need to try it. I think this is possible, but will take more time. And more frequent shaking and possibly additional heating. But I think this is possible. We can replace HBr, but it will be a different method.

 

[animeboro]

12% perhydrol works, but you need to use much more of it. The cheapest way to buy hbr in taiwan is as much as hcl

 

[dnBQByvHb8Zkawbjpx]

The cheapest is not always the best. As an individual consumer in the EU with no registered business I'd have a hard time explaining the import of HBr to the customs in case they ask. Extraction from pool chemicals seems to be the only reasonable way to someone like me buy I have yet to do that myself.

 

[WillD]

If you can buy BK, then part of the problem is solved. If not, then you can use other methods of bromination or iodination.

 

[WillD]

As an example, boiling with CuBr2 in ethylacetate, separate from the sediment, and then everything will be the same (starting from the reaction with methylamine). For boiling ethylacetate enough hot water in a pan, if we adhere to the "Voss" synthesis

 

[animeboro]

instead of methylamine water solution, it is better to use methylamine hcl with naoh then your clothes won't stink like fish and you can work without a gas mask

 

[Dr. MMX]

its not better, its only better if you cant prepare solution urself and you dont have access to good quality ma 40% and ur working in the small scale

 

[WillD]

The use of methylamine hydrochloride is not suitable for this synthesis. Unless you get an alcohol solution without sodium hydroxide.

 

[Dr. MMX]

12% does work too. However remember that in the bromination most important is enolization, its the beggining of the reactiobn. h2o2 can be strange sometimes and it may lead to not react bromine at all enolization occurs in lower temperatures, so if you have the way you can cool a little solution and slowly heat it up later. In every case lower temp is a lot of better for this. Br behavior is precise attack into the correct place where you want it to be, without enolization is a full lose

 

[animeboro]

I would do it like this we get 4methylenopropiophenone per 100ml 150g 2b4m used 750ml ethyl acetate methylamine hcl 195g/naoh 105g+distilled water 150ml rinse 3 times with distilled water, 450 ml each (total 1.4 l) and hbr acid to pH 5 if the powder is brown, use water and NACI salt, heat the whole thing and put it in the freezer at -18°, then the whole NaCI will remove the dirt crystallization mmc powder + tap water or tap water and ipa 1g mmc to 0.8ml of water heat the saturated solution slightly, set aside at room temperature and the next day we have a crystal or use 1g of powder 0.8ml tap water and 0.2ml ipa and do the same as with just water

 

[animeboro]

It would be nice to show the yield of this synthesis on a scale so that everyone would not have to ask whether the synthesis is good or not, just because it is produced does not mean that it is the best.

 

[Dr. MMX]

"best" can be only usage of knowledge in this reaction and its conditions should be estabilished based on the situation and possibilities to perform. If you do good you will always receive pure product, without any need of futher purification

 

[Dr. MMX]

you can buy it on allegro, they dont check anythinfg they just send 35 %

 

[dnBQByvHb8Zkawbjpx]

I prefer not to poke this bear. According to the EU regulation sellers are to report suspicious purchases, including attempted ones. I don't need to end up on any more lists.

 

[abis777]

Is only 12%

 

[animeboro]

crystallization of 2b4m, add dcm or ethyl acetate to the 2b4m powder, heat the whole thing until all the 2b4m dissolves and put it in the freezer overnight and a clean 2b4m glass is created, but it works best in dcm proportions 1g 2b4m powder per 0.8ml dcm saturated solution similar to mmc crystallization

 

[Dr. MMX]

you cant use dcm for crystalisation.. i mean you can but you must wash it with acetone later. Why use dcm at all?
Water and if product isnt pure, then add some ipa alcohol to help crystals grow.