Bromine

[TheVacuumGuy]

gives opportunity to make 4-MMC to every beginner of organic synthesis.​

(maybe a warning would be "nice") regarding benzene / bromine
These are nearly impossible to obtain. Well, with business registration and documents it is possible, but i'll skip for now (business just 2 weeks old).

As i spent a shitload of money already to buy equipment, there is not really a way back but to make it myself (Bromine).

Now i see al those video's full of dangerous fumes and heavy ventilation system, warnings and so on, but i stubled upon this one below.

I'm curious, it almost seems like this way i can get my bromine by just getting the top layer out using a pipette or something wihout "too much danger"

Any experience anyone? Is this viable? Also when using NaBr instead of Potassium Bromide?

https://imgur.com/a/xHw0vMD

 

[SonicNL]

Cant you skip this step and buy a brominated precursor?

 

[TheVacuumGuy]

Yes sure, but got quite an amount so after that it would certainly be an option. Although Im not sure if thats much easier. Time and learning curve will tell

 

[BitcoinScam]

Yes sure, but got quite an amount so after that it would certainly be an option. Although Im not sure if thats much easier. Time and learning curve will tell

TheVacuumGuyif u are from europa i can buy easy brom or Hbr with perhydrol much more easy made like i on video

 

[TheVacuumGuy]

if u are from europa i can buy easy brom or Hbr with perhydrol much more easy made like i on video

BitcoinThanks. I'll remember that for later use. I can also buy the end product directly, but that defeats the purpose of this endeavour a bit.

 

[BitcoinScam]

Thanks. I'll remember that for later use. I can also buy the end product directly, but that defeats the purpose of this endeavour a bit.

TheVacuumGuywhy if you buy a lot 2b4m they give u good price. The same if u made 100kg u dont need use reactor 100l in my country they use mauzer 1000l and they mix all together and they get crystal like ice.

 

[TheVacuumGuy]

why if you buy a lot 2b4m they give u good price. The same if u made 100kg u dont need use reactor 100l in my country they use mauzer 1000l and they mix all together and they get crystal like ice.

BitcoinIdc about price but these are numbers which are not even a goal for me. I'm going for my first try in chemistry. I'd be more happy with 250g selfmade excellent quality (someday) than 100kg of whatever some stranger "mixed all together".
But thanks anyway

 

[auc]

Yo empecé a producirlo y el proceso es medio fácil pero sostenerlo sin que se evaporara es difícil y cada vez que lo hacia lo metía al congelador para que no se evaporara tan fácil.

Después de un tiempo me aburrí y logre que una empresa me lo importe y compre 2 litros y me dura demaciado.
solo que es difícil mantenerlo controlado

 

[BitcoinScam]

Yo empecé a producirlo y el proceso es medio fácil pero sostenerlo sin que se evaporara es difícil y cada vez que lo hacia lo metía al congelador para que no se evaporara tan fácil.

Después de un tiempo me aburrí y logre que una empresa me lo importe y compre 2 litros y me dura demaciado.
solo que es difícil mantenerlo controlado

aucenglish bro

 

[TheVacuumGuy]

To answer this: it kind of works, but looks far from "usable"

 

[w2x3f5]

You can get bromine from hydrobromic acid with hydrogen peroxide (the oxidizing agent can be another oxon and the like), you can get it from metal bromides with reactions of sulfuric acid plus an oxidizing agent. In most reactions, bromine can be obtained directly during the reaction without isolating it in its pure form, a very unpleasant substance.

 

[TheVacuumGuy]

Yesterday I tried something which seems promising using potassium bromide, sodium hypochlorite and HCl.

 

[w2x3f5]

Yesterday I tried something which seems promising using potassium bromide, sodium hypochlorite and HCl.

TheVacuumGuyAll hypochlorite solutions are stabilized with sodium hydroxide; this unpleasant point must be taken into account. You are using a very inconvenient oxidizing agent.
you can try phosphoric acid or sulfuric acid, hydrochloric acid is not the best option since they can oxidize to chlorine the moment the bromide runs out.

 

[WillD]

maybe NBS is possible for u? CuBr2 also is possible. CuO/iodine system. H2O2/HBr system (my favorite choice)

 

[TheVacuumGuy]

maybe NBS is possible for u? CuBr2 also is possible. CuO/iodine system. H2O2/HBr system (my favorite choice)

William DampierThanks!
If i understand correctly, i could brominate directly using N-Bromosuccinimide as substitute for br2? That would save a tremendous amount of work + easy to obtain.

 

[w2x3f5]

Thanks!
If i understand correctly, i could brominate directly using N-Bromosuccinimide as substitute for br2? That would save a tremendous amount of work + easy to obtain.

TheVacuumGuyThe NBS bromination catalyst is Tos acid, the reaction is very fast, selective and clean. NBS is expensive compared to other bromine sources.

 

[TheVacuumGuy]

The NBS bromination catalyst is Tos acid, the reaction is very fast, selective and clean. NBS is expensive compared to other bromine sources.

w2x3f5too late. 500g is on its way. what is Tos acid btw?

 

[w2x3f5]

too late. 500g is on its way. what is Tos acid btw?

TheVacuumGuy

p-Toluenesulfonic acid​

 

[41Dxflatline]

KBr is widely available (NaBr I don't know). Just add some conc. sulfuric acid and get set up for vacuum distillation. Slowly add in H2O2 with an addition funnel. Once done take a sep funnel and add a little conc. h2so4, pour your bromine+water solution into the sep funnel, extract the bottom layer into a test tube and seal with a blowtorch. The most dangerous part is adding the liquid to the sep funnel.

 

[TheVacuumGuy]

KBr is widely available (NaBr I don't know). Just add some conc. sulfuric acid and get set up for vacuum distillation. Slowly add in H2O2 with an addition funnel. Once done take a sep funnel and add a little conc. h2so4, pour your bromine+water solution into the sep funnel, extract the bottom layer into a test tube and seal with a blowtorch. The most dangerous part is adding the liquid to the sep funnel.

41DxflatlineYeah that's all over YouTube as well. H2O2 is restricted here so hard to get besides purifying . I found some which I'm still waiting for but only 35%