My 3-CMC synthesis:
at first i want to thank William Dampier for his advices.
I use a sealed glass with a thick toppits foil between lid and glass to prevent fumes.
And no, it will NOT explode, if you use this kind of glass.
I tried with dcm and ethylacetate and both works fine.
The benefit of ethylacetate is the short cooking time, about 20 min.
You do not have to heat it till above 35 degress like with dcm.
But the layers are opposite, water down in ethylacetate and dcm up.
For example:
100g 2b3c
300 dcm
200 methylamin40% aqua
3 hours at aprox 36 degrees
20 min with ethylacetate
After that, open the glass and put same amount as rm, icecold,dest.water /10% sodium bicarbonate inside, this is the first wash to get rid of methylamine.
2 additional washing with dest.water
(same amount as rm)
extract both 2 last washings(water layer) with dcm to get rest of freebase,
then put into rm.
After that, add same amount fresh, cold dest.water into rm, let it stir some time.
Then separate organic and water layer.
I tried different kind of acidificaction.
organic layer alone and organic/water layer together.
I prefer the second one.
Organic layer will be disposed in this case.
put on magnetic stirrer
for acidificaction i use dripping or separatory funnel, drop by drop
(every 2-3 seconds)
till ph6, about 40ml 37% HCI
(i do not mix it with acetone)
While acidificaction the rm begins to change its color from yellow to orange.
After that, separate the water layer with a separatory funnel, put it into a bowl or dish, let it crystallize, this will take some time, 2-3 days.
Freezer gave me strange results so i do not recomend it.
After the crystals have formed, i had different results, sometimes very clear, sometimes light yellow.
So, to get them clear as possible, you have to crush them to powder, wash with acetone, filter with buchner.
Put the acetone into a bowl and let it evaporate, there will be some rest of powder mostly, that will be crushed and washed again.
The washed powder from buchner will be dried and we recrystallize it again.
300ml beaker, 1ml dest.water per 1g powder heated on magnetic stirrer till 60/70 degrees.
Then put Powder into the beaker, let it dissolve and stir 1-2 min.
Then put 2ml ipa or acetone per 1g powder into the beaker, let it stir a short time.
After that, put again into a bowl or dish, evaporate and crystals will form.
Repeat this step until you got the clearness which you want to have.
About the yield (aprox 30-40%, at first i only had about 20%, because i did not re-use the solution after crystalisation), to be honest, i expected more, but maybe my synthesis has some issues or something happened i do not know.
If someone has better experiences, please share your knowledge.
As far as i see here in the forum, many people have questions about 3-cmc but good and helpful answers are hard to find.
The pictures are from different batches and different stages.
at first i want to thank William Dampier for his advices.
I use a sealed glass with a thick toppits foil between lid and glass to prevent fumes.
And no, it will NOT explode, if you use this kind of glass.
I tried with dcm and ethylacetate and both works fine.
The benefit of ethylacetate is the short cooking time, about 20 min.
You do not have to heat it till above 35 degress like with dcm.
But the layers are opposite, water down in ethylacetate and dcm up.
For example:
100g 2b3c
300 dcm
200 methylamin40% aqua
3 hours at aprox 36 degrees
20 min with ethylacetate
After that, open the glass and put same amount as rm, icecold,dest.water /10% sodium bicarbonate inside, this is the first wash to get rid of methylamine.
2 additional washing with dest.water
(same amount as rm)
extract both 2 last washings(water layer) with dcm to get rest of freebase,
then put into rm.
After that, add same amount fresh, cold dest.water into rm, let it stir some time.
Then separate organic and water layer.
I tried different kind of acidificaction.
organic layer alone and organic/water layer together.
I prefer the second one.
Organic layer will be disposed in this case.
put on magnetic stirrer
for acidificaction i use dripping or separatory funnel, drop by drop
(every 2-3 seconds)
till ph6, about 40ml 37% HCI
(i do not mix it with acetone)
While acidificaction the rm begins to change its color from yellow to orange.
After that, separate the water layer with a separatory funnel, put it into a bowl or dish, let it crystallize, this will take some time, 2-3 days.
Freezer gave me strange results so i do not recomend it.
After the crystals have formed, i had different results, sometimes very clear, sometimes light yellow.
So, to get them clear as possible, you have to crush them to powder, wash with acetone, filter with buchner.
Put the acetone into a bowl and let it evaporate, there will be some rest of powder mostly, that will be crushed and washed again.
The washed powder from buchner will be dried and we recrystallize it again.
300ml beaker, 1ml dest.water per 1g powder heated on magnetic stirrer till 60/70 degrees.
Then put Powder into the beaker, let it dissolve and stir 1-2 min.
Then put 2ml ipa or acetone per 1g powder into the beaker, let it stir a short time.
After that, put again into a bowl or dish, evaporate and crystals will form.
Repeat this step until you got the clearness which you want to have.
About the yield (aprox 30-40%, at first i only had about 20%, because i did not re-use the solution after crystalisation), to be honest, i expected more, but maybe my synthesis has some issues or something happened i do not know.
If someone has better experiences, please share your knowledge.
As far as i see here in the forum, many people have questions about 3-cmc but good and helpful answers are hard to find.
The pictures are from different batches and different stages.
