question about 3cmc synth

[draconic123]

hello people, so i've been doing 3cmc synth with ethyl acetate and i'm acidifying freebase with water, 3cmc doesnt precipitate when acidifying freebase only for some reason... regardless, i was wondering whether it would be possible to add IPA before acidification in order to get clean crystals in one go, or would it ruin the reaction?

 

[The-Hive]

Acetone/Hci or IPA

 

[Jesse_Pinkman_]

It does not fall out while acidification...
The crystals form while evaporation from the water layer.

 

[Jesse_Pinkman_]

I had also results with acidification in freebase only but were not as good as with water together and evaporate the water layer.
Recrystallisation after acidification should be possible but if the crystals are cleaner then, i can not say.

 

[draconic123]

I had also results with acidification in freebase only but were not as good as with water together and evaporate the water layer.
Recrystallisation after acidification should be possible but if the crystals are cleaner then, i can not say.

Jesse_Pinkman_Have you ever tried reaction with 2 solvents? Im gonna buy some nmp and try with nmp and ethyl acetate.. should be much more clean and more crystals

 

[Bazooka90]

op

hello people, so i've been doing 3cmc synth with ethyl acetate and i'm acidifying freebase with water, 3cmc doesnt precipitate when acidifying freebase only for some reason... regardless, i was wondering whether it would be possible to add IPA before acidification in order to get clean crystals in one go, or would it ruin the reactio

draconic123What temperature did u use for ethyl acetate reaction?

 

[Jesse_Pinkman_]

op

What temperature did u use for ethyl acetate reaction?

Bazooka90No temp control needed, just mix and stir for 20min... temp rises and falls from the reaction itself

 

[BitcoinScam]

No temp control needed, just mix and stir for 20min... temp rises and falls from the reaction itself

Jesse_Pinkman_how much u get gram 3cmc form 2b3ch if u use ethyl acetate

 

[The-Hive]

how much u get gram 3cmc form 2b3ch if u use ethyl acetate

BitcoinFor every 100g you should get 75-80g 3cmc

 

[Jesse_Pinkman_]

how much u get gram 3cmc form 2b3ch if u use ethyl acetate

BitcoinNot very much, 30-40% max.

 

[Jesse_Pinkman_]

how much u get gram 3cmc form 2b3ch if u use ethyl acetate

BitcoinHow do you get this result?

 

[BitcoinScam]

How do you get this result?

Jesse_Pinkman_on dcm

 

[Jesse_Pinkman_]

on dcm

BitcoinEven with DCM i only got 40% yield...

 

[BitcoinScam]

Even with DCM i only got 40% yield...

Jesse_Pinkman_do u heat it ?

 

[BitcoinScam]

Even with DCM i only got 40% yield...

Jesse_Pinkman_how much dcm u use ?

 

[Jesse_Pinkman_]

do u heat it ?

BitcoinYes, heat until 36 degrees
300ml per 100g 2b3c

 

[BitcoinScam]

Yes, heat until 36 degrees
300ml per 100g 2b3c

Jesse_Pinkman_I've already answered the question myself: one, the temperature is too low, two, the proportions are wrong and there are probably other errors along the way, that's why you have such results

 

[Jesse_Pinkman_]

I've already answered the question myself: one, the temperature is too low, two, the proportions are wrong and there are probably other errors along the way, that's why you have such results

BitcoinCould you give me an advice, how you do it?

 

[BitcoinScam]

Could you give me an advice, how you do it?

Jesse_Pinkman_ask expert on this forum

 

[The-Hive]

Probs to much water init

 

[The-Hive]

hello people, so i've been doing 3cmc synth with ethyl acetate and i'm acidifying freebase with water, 3cmc doesnt precipitate when acidifying freebase only for some reason... regardless, i was wondering whether it would be possible to add IPA before acidification in order to get clean crystals in one go, or would it ruin the reaction?

draconic123Upload the synthesis your following

 

[draconic123]

Upload the synthesis your following

The-HiveIm doing what jesse pinkman is doing in his post except im adding 5:1 ratio of ethyl acetate to 2b3c, im thinking of acidifying rm with less water and some ipa because right now I add same amount as rm and clearly its too much and slows down crystalization