Synthesis 4mmc with ethyl acetate in 20min

[Chemix-Express]

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

 

[TheVacuumGuy]

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

Chemix-ExpressNot 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

 

[Mellym]

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.

 

[StarWars]

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:
View attachment 9085

After about 30min. not much had changed:
View attachment 9086
At this moment I decided to heat things up . Not higher about 50-55C.

One hour later:
View attachment 9087
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.
View attachment 9090 View attachment 9091 View attachment 9092
And that gave raw product. Rather nice at first sight, but should be further purified, of course.

MellymU use to much ethyl acetate u need use only 100ml no 250ml

 

[TheVacuumGuy]

U use to much ethyl acetate u need use only 100ml no 250ml

StarWarsYep. 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