any 3CMC synthesis method?

[rafael1985]

Procedure was the same like with 4 mmc but I put I think too much 35% HCL is possible to rescue this only is nothing

 

[rafael1985]

pH is 2 really acid

 

[G.Patton]

5-5.5 is optimal pH, but there is a lot of watery HCl acid and 3MMC salt precipitation would dissolve in water

 

[rafael1985]

What I must do try evaporate this water when I put to freezer nothing come.Or maybe put acetone and use freezer.Or maybe try put sodium carbonate make pH higher will be work?

 

[G.Patton]

You have to alkalize your solution to pH 12-13, extract 3MMC free base by ether or petroleum ether and then add HCl gas to acidify solution. You'll get 3MMC salt precipitate.

 

[Lucy123]

Did You manage to get the 3cmc? Would it work If I follow the same steps as for the 4cmc with 3-chloropropiophenone?

 

[G.Patton]

I think yes, this molecule has almost the same properties.

 

[rafael1985]

I make every steps like bromination 4 MMC on dichlorometane but I start from oil and after acidification i let in room temp and nothing come only water again somebody know how to make crystalization process?Is different like with 4 MMC

 

[G.Patton]

Have you tried what I suggested?

 

[rafael1985]

I must alkalize this with sodium hydroxide?

 

[G.Patton]

yes, you can take 20% aq solution

 

[rafael1985]

Is anybody here have success with synthesis 3 cmc with good yield?

 

[Bazooka90]

my 3cmc yield is very brownish,does anybody know how to make it more white?can i use some bleach?

 

[Jesse_Pinkman_]

Crush it to powder, wash with icecold acetone, then recrystalisation with dest water/ipa , dest water/acetone or just Methanol (5ml per 1g Powder).
Some use only water but this takes more time to evaporate

 

[rafael1985]

I have problem to make powderAfter acidificarion is nothing come.I put to frezer with acetone nothing come after evaporate is Black gum.PH is good.With 4 MMC and 4 CMC was not problem.Can You help somehow?

 

[Jesse_Pinkman_]

After acidification you have to separate the organic from water layer and put the water layer in some dishes/containers and let them stand for some days, sometimes +1 week, depends on volume.
Crystals begin to form when 50% have evaporated.
When crystals have stopped forming and they are not clean, you have to crush them to powder with a mixer, wash with icecold acetone, dry and then do recrystalisation with dest water/ipa or only Methanol or dest water/acetone.

 

[G.Patton]

Have you seen my topic? Home purification method for mephedrone You can purify it easy by the same way.
There is too much water, I think. You have to get rid of water. I told you how to deal with it.

 

[The-Hive]

@Berlin777 check this out

 

[Berlin777]

thanks for that The-Hive, decided not to try acetone way when it comes to 3CMC, it would be inefficient

 

[The-Hive]

Good idea let us know the results