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madmoney69

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who finished this synth successfully?
 

darkblink

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What equipment is used for large scale production? im currently using 1000ml glass flasks for small amounts, anything metal reacts with the solution, i was thinking of using ceramic 6.5 litre slow cooker pot, mechanical stirrer and a plug in temperature control thermostat to controll temp.
 

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Can anyone recommend a supplier of NMP to the UK?
 

WhalterWhite

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Hello. I have 100 l liquid 2bromo3chloro.. , toulen , and replace Dmso Sulfolane. I try start do 3cmc.


When doing 3cmc all the steps are the same? On the forum they write that yes but I prefer to ask. So far I have done 4mmc without salivation. I mixed 2h at 40 degrees 2b4met with methylamine and toulene. Finally, I poured water with acid, separated the layers and I dry for about a week and wash with acetone and ihad 50% efficiency of 4mmc powder. Now I would like to try your recipe.

One more question. Once, a salesman instead of toulen sold me dichloromethane. However, the mephedrone layer does not come out on top of this. Is dichloromethane useful for anything? Sorry for my English, it's poor
 
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Venom2021

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methylene chloride is better in my opinion at 4mmc true 2h 40 ° but with 40 ° taulen it is too small the temperature must be higher than 50%, i.e. 100g bk4 50g 4mmc + a lot of impurities because you do not clean the oil at all I see after crystallization you will have somewhere 40g maybe less efficiency I obtained 70% and 80% yield on methylene chloride
 

Epikureetsdrug

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methylene chloride is better in my opinion at 4mmc true 2h 40 ° but with 40 ° taulen it is too small the temperature must be higher than 50%, i.e. 100g bk4 50g 4mmc + a lot of impurities because you do not clean the oil at all I see after crystallization you will have somewhere 40g maybe less efficiency I obtained 70% and 80% yield on methylene chloride
Venom2021my respect! could you share your unique experience of obtaining 70% yield in the synthesis of 4mmc in DCM? This is an extremely interesting result, at least for me. I will be very grateful to you for the enlightenment.
 

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you're right. After crystallization, I was left with 40%. And when I tried to salt the solution with caustic soda once, I had 23% efficiency left.
As for chloromethane, at 40 ° C, two layers separated with stirring for two hours. However, after 10 minutes, the color was the same and there were no two layers. Can I also use chloromethane in 3cmc?
 

Venom2021

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For 4cmc the process should be the same 3cmc I did not do After 60% crystallization, this is the minimum
 

rafael1985

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With 3 cmc every step are the same but after acidification with HCl 35-37% product is liquid form.You must evaporate water but is really dirty black product.With 2 bromo 4 chloro or methylo You dont have problems like with this 2 bromo 3 chloro liquid
 

rafael1985

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you're right. After crystallization, I was left with 40%. And when I tried to salt the solution with caustic soda once, I had 23% efficiency left.
As for chloromethane, at 40 ° C, two layers separated with stirring for two hours. However, after 10 minutes, the color was the same and there were no two layers. Can I also use chloromethane in 3cmc?
WhalterWhiteMaybe You put to less methylamine.
For 1 kg ketone nie much You give methylamine?
 

WhalterWhite

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Can You tell how You make powder You put cold acetone HCl and let on freezer ?
rafael1985I didn't give to freezer. I waited and the substance will dry out which took time. Then I rinsed with acetone and there was powder. I did according to my own recipe. Now I want to try 3cmc with a refrigerator to speed up the process
 

rafael1985

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I didn't give to freezer. I waited and the substance will dry out which took time. Then I rinsed with acetone and there was powder. I did according to my own recipe. Now I want to try 3cmc with a refrigerator to speed up the process
WhalterWhiteWith 3 cmc you will be have more fun
 

Epikureetsdrug

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With 3 cmc you will be have more fun
rafael1985I totally agree with you, friend. 3cmc somehow reminded me of a-pvp in terms of the method of isolation and crystallization. Due to the water in which hydrogen chloride is dissolved, they do not immediately crystallize from the solvent, but settle to the bottom in the form of an oily liquid. a-pvp is red, and 3cmc is radically black. Therefore, it is necessary to carefully decant the upper layer of the solvent and then rinse that viscous liquid with a fair amount of acetone, and almost immediately the substances precipitate. it remains only to filter and recrystallize.
 
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