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??
Synthesis 4mmc with ethyl acetate in 20min
- Thread starter StarWars
- Start date
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 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.
Attachments
- By StarWars
U use to much ethyl acetate u need use only 100ml no 250ml
- By TheVacuumGuy
Yep. Unlike other solvents which you can roughly use a x 3 amount, this one is x 2.
100g ketone
200ml ethyl acetate
200ml methylamine
No heat is bs, just gentle heat rm 30c
Add amine, no need for dropwise, just add it straight, but not overdo it.
Temp will rise to 50/60 and cool down slowly. Colors are light yellow , darker yellow, cleared up yellow, cleared up deep dark yellow. Done
Very nice route to go for, no amine smell like DCM, and can be disposed in toilet.
I do it even in living room couple times no problem
100g ketone
200ml ethyl acetate
200ml methylamine
No heat is bs, just gentle heat rm 30c
Add amine, no need for dropwise, just add it straight, but not overdo it.
Temp will rise to 50/60 and cool down slowly. Colors are light yellow , darker yellow, cleared up yellow, cleared up deep dark yellow. Done
Very nice route to go for, no amine smell like DCM, and can be disposed in toilet.
I do it even in living room couple times no problem
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