hello, I am interested in the synthesis of 4mmc with bk4 and ethyl acetate and M40%. Why is it so short only 20min mix\shake? Why is it not heated? what purity can be achieved?? can you make it in a closed borosilicate bottle and shake it??
Synthesis 4mmc with ethyl acetate in 20min
- Thread starter StarWars
- Start date
Because it is enough to convert bk4 to 4-MMC. You can check a reaction readiness by TLC. You can reach 98+% purity by recrystallization. You have to keep system opened to avoid explosion.
I made such tests with toluene and dcm and it did not explode, why should it explode with ethyl acetate??
Br2 forms during this reaction. When volume of Br2 too big, reaction stops.
- By StarWars
Then u use toulen benzen dcm is not the same like on ethyl acetate??
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- By StarWars
I was use dcm and in shake 10min temprature i get 36°c and im do it with bottel because one guy say is also good and later i was heat 2h 40C and im shake sometime and not Explode and im use
1kg bk
2l m40
2l dcm
Later when im finish cook im wash water and later IPA and HCl and all go good
Tell me why can explote because still im not Understend when i made the same like on video where there he have close glass the same like im can use bottel and shake is the same like im use stirrer.
1kg bk
2l m40
2l dcm
Later when im finish cook im wash water and later IPA and HCl and all go good
Tell me why can explote because still im not Understend when i made the same like on video where there he have close glass the same like im can use bottel and shake is the same like im use stirrer.
Do I understand correctly? You give 1kg bk4, 2L m40, 2L dcm. The temperature in 10 minutes automatically rises to above 36 degrees, then you turn on the heating on the stirrer and so you mix 2 hours at 40 degrees, right?
I have a couple of fundamental questions:
1. we don't heat the whole thing to 40 degrees before adding the m40, and we add all the m40 at once?
2. there is no need to watch the temperature when adding m40?
3. can I use HCL + IPA for acidification instead of hcl + acetone? Want to get rid of unnecessary colour when acidifying.
4. the yield came out lower due to using iodo ketone, with bk4 it should be better?
5. in the forum video it says that the reaction ends when the base is brown, with bk4 also? Or is there another way to confirm that the whole has gone fully?
Thanks for your time
1. we don't heat the whole thing to 40 degrees before adding the m40, and we add all the m40 at once?
2. there is no need to watch the temperature when adding m40?
3. can I use HCL + IPA for acidification instead of hcl + acetone? Want to get rid of unnecessary colour when acidifying.
4. the yield came out lower due to using iodo ketone, with bk4 it should be better?
5. in the forum video it says that the reaction ends when the base is brown, with bk4 also? Or is there another way to confirm that the whole has gone fully?
Thanks for your time
- By G.Patton
Hello, ask your question about this synthesis in appropriate topic please. It isn't synthesis topic.
Depends on scale and reaction temperature. Avoid overheating.
yes, you can use dry IPA but it worth to use acetone.
almost the same
Have you seen video tutorials? Yes, TLC can be used.
Depends on scale and reaction temperature. Avoid overheating.
yes, you can use dry IPA but it worth to use acetone.
almost the same
Have you seen video tutorials? Yes, TLC can be used.
- By TheVacuumGuy
Not trying to correct you, but learning and trying equations at the moment. So could you confirm following:
C10H11BrO + CH3NH2 = C11H15NO + HBr
Which would mean HBr is forming as Br2 is diatomic ?
Chemix sorry this was question for G.patton
C10H11BrO + CH3NH2 = C11H15NO + HBr
Which would mean HBr is forming as Br2 is diatomic ?
Chemix sorry this was question for G.patton
For those who is interested. I've tried this route. Overall I can confirm it works, except reaction conditions. Temperature and timing were not even close as it's stated in video. Though, in the video they use Iodo-ketone. That's a significant difference.
So, the test run I got 50g of bromine substituted 4-MPF. That was dissolved in 250ml of ethylacetate
than 100ml of aq. 38% methylamine was added. and left to stir at room temp:
After about 30min. not much had changed:
At this moment I decided to heat things up . Not higher about 50-55C.
One hour later:
It was showing some movement. And was left for another hour.
Then basically the steps were the same as in video. Ethylacetate layer with freebase was separated, washed with water, HCL added dropwise until slightly acidic pH. Then acetone poured and filtered.
And that gave raw product. Rather nice at first sight, but should be further purified, of course.
So, the test run I got 50g of bromine substituted 4-MPF. That was dissolved in 250ml of ethylacetate
than 100ml of aq. 38% methylamine was added. and left to stir at room temp:
After about 30min. not much had changed:
At this moment I decided to heat things up . Not higher about 50-55C.
One hour later:
It was showing some movement. And was left for another hour.
Then basically the steps were the same as in video. Ethylacetate layer with freebase was separated, washed with water, HCL added dropwise until slightly acidic pH. Then acetone poured and filtered.
And that gave raw product. Rather nice at first sight, but should be further purified, of course.
