Meow Meow "Voss" synthesis

[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 %?

 

[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

 

[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

 

[animeboro]

brown mmc powder is created when we add the acid too quickly and the freebase starts to overheat, then all the pyrizine and other impurities start to come out, which means that we have lower efficiency. the same way we clean the wrong MMC free base, I use water and water with baking soda 3 times and water with baking soda always saves my life even when the entire solution did not react after rinsing with water and baking soda, I get the free base from the green oil of the MMC free base to yellow, changing the color green to blue and then to yellow

 

[dnBQByvHb8Zkawbjpx]

When you talk about overheating, what temperature are you actually talking about? The last time I did acidification I had a thermometer in the RM and it finished just above 0 °C.

 

[WillD]

We can all rush, especially when the product is needed now But we can speed up the process of acidification with compulsory cooling, for example in a pan with cold water.

 

[WillD]

We can use HCl acid for this method, no problems. But in this case, we wanted to use HBr, soon you will see why.

 

[animeboro]

from what I noticed, washing with water alone sometimes does not help at all, in many cases soda and water cleans 100% solution, you should even do extraction, e.g. with DCM, to further clean the free base as much as possible, you can also use NaCi to displace all the water from the free base and use hbr, but can hbr has water in it like hcl??

 

[Dr. MMX]

Why do you suggest to do that?
Simply aquenous layer is just removed and product washed when its properly performed. Providing another extractions will only complicate it and its no needed.

 

[WillD]

Yes, there is water there. But in this synthesis, we need water, soon you will find out why. This is for crystallization. The brine can be used when you wash the reaction for better separation of the organic layer.

 

[animeboro]

Tap water is best for crystallization, it gives pure crystals like icicles. I used demineralized distilled water and it did not give the same effect as regular tap water.

 

[animeboro]

My crystal was the same like crystal this seller for uk

 

[WillD]

I heard about this. Perhaps mineral components in tap water are given crystallization centers.

 

[Dr. MMX]

I believe it does help to form them. But I dont agree that tap water will be better than distilled. Simnply the temperature must be very carefully dropped down to form 1st crystals (even sometimes it can be incrashed a bit to decrashe it again to receive nice nick in to 1st crystals that will appear, it will modify its shape.). Crystalisation can be finished in less than 2h receiving such result with about 60-65% powder's weight from mother liquior, then repeated and the about last remaining 5% should be left to be just drippefd with acetone lightly. of course its estimated grams. But I believe 60-65% for mother liquior is very good score (till 25c)

 

[animeboro]

Total how much gram get mmc ?? And how look crystal when dry ?

 

[animeboro]

My 2bromo4methylenopropiophenone i thing looks no so bad
170g form 100ml 4-Methylonepropiophenone

 

[animeboro]

4-methylenopropiophenone 100ml 40pln
Hbr 48% 75ml 40pln
100ml perhydrol 12% 4 PLN
Ethyl acetate 100ml 3pln
= 87 PLN 170g
100g 2b4m 51.17pln

 

[WillD]

This is all wonderful, but in theory you cannot get more than 150g with 100mL. Excess weight is moisture from the reaction (or dibromine derivatives). If you are talking about the weight of the final product, then the formation of crystalline hydrates is possible.

 

[animeboro]

pH which was 4 then I purified water and baking soda and then crystallized with ethyl acetate