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any 3CMC synthesis method?

rafael1985

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

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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?
rafael1985You 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.
 
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Lucy123

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You have to alkalize your solution to pH 12-13, extract 3MMC free base by ether or petroleum ether and than add HCl gas to acidify solution. You'll get 3MMC salt precipitate.
G.PattonDid You manage to get the 3cmc? Would it work If I follow the same steps as for the 4cmc with 3-chloropropiophenone?
 

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rafael1985

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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
 

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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
rafael1985Have you tried what I suggested?
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.
 

rafael1985

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I must alkalize this with sodium hydroxide?
 

rafael1985

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

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

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my 3cmc yield is very brownish,does anybody know how to make it more white?can i use some bleach?
Bazooka90Crush 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

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my 3cmc yield is very brownish,does anybody know how to make it more white?can i use some bleach?
Bazooka90I 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?
 

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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?
rafael1985After 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.
 

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G.Patton

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my 3cmc yield is very brownish,does anybody know how to make it more white?can i use some bleach?
Bazooka90Have you seen my topic? Home purification method for mephedrone You can purify it easy by the same way.
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?
There is too much water, I think. You have to get rid of water. I told you how to deal with it.
 

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Good idea let us know the results
 
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