Synthesis 4mmc with ethyl acetate in 20min

[StarWars]

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??

 

[G.Patton]

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.

 

[StarWars]

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.

G.Pattonit can explode if the temperature of the solution significantly exceeds the boiling point of the diffuser, am I right??

 

[StarWars]

I made such tests with toluene and dcm and it did not explode, why should it explode with ethyl acetate??

 

[G.Patton]

Br2 forms during this reaction. When volume of Br2 too big, reaction stops.

 

[StarWars]

Br2 forms during this reaction. When volume of Br2 too big, reaction stops.

G.PattonThen u use toulen benzen dcm is not the same like on ethyl acetate??

 

[G.Patton]

Then u use toulen benzen dcm is not the same like on ethyl acetate??

StarWarsSolvent doesn't play role. Br2 is released according reaction equation.

 

[StarWars]

Then u use toulen benzen dcm is not the same like on ethyl acetate??

StarWarsI 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.

 

[G.Patton]

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.

StarWarsThe pressure of Br2 won't be too height to explode the bottle, probably I was wrong, but be careful. Better to use open system with reflux condenser.

 

[Chemix-Express]

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.

StarWarsDo 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?

 

[Chemix-Express]

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.

StarWarsAcidify with hydrochloric acid in IPA instead of acetone?

 

[StarWars]

Acidify with hydrochloric acid in IPA instead of acetone?

Chemix-ExpressYes.
With ethyl acetate will be faster like on video 20min

 

[StarWars]

Acidify with hydrochloric acid in IPA instead of acetone?

Chemix-ExpressU can use ethyl acetate and HCl also

 

[Zarder]

I’m sorry but what is bk?

 

[HairyPoppins]

I’m sorry but what is bk?

ZarderBromo Ketone

 

[StarWars]

Bromo Ketone

HairyPoppinsYes

 

[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

 

[G.Patton]

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-ExpressHello, ask your question about this synthesis in appropriate topic please. It isn't synthesis topic.

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?

Depends on scale and reaction temperature. Avoid overheating.

3. can I use HCL + IPA for acidification instead of hcl + acetone? Want to get rid of unnecessary colour when acidifying.

yes, you can use dry IPA but it worth to use acetone.

4. the yield came out lower due to using iodo ketone, with bk4 it should be better?

almost the same

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?

Have you seen video tutorials? Yes, TLC can be used.

 

[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.

Mellymthe flask should be tightly closed and should be stirred vigorously

 

[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