I trying 4mmc?

[Toddler]

plz check the whole process and plz tell me which step i do mistake, mixture not perform white Flappy liquid.


20g 2b4m
100ml EA
stirrer until dissolve,
Then add 40ml MA 40%.

stirrer 1 hours temp not goes above 30.2. Without water bath.

then put in separating funnel.
first wash once with bicarbonate 5% 60 ml solution,

then 3 time wash with cold water 60ml x 3 times

After wash add 200ml chilled acetone.
Then dropping add hcl 33%.

After some add hcl color change yellow to brown.
Then

after some drop like 3-4 drop add hcl
change brown to green

after some time without dropping hcl color change to yellow.
But not performing white liquid.
As all saying

 

[Toddler]

@G.Patton @William D. @HIGGS BOSSON @Marvin "Popcorn" Sutton @TheVacuumGuy @Dr. MMX @GhostChemist @HEISENBERG

All other plz help me.

thankyou in advance.

 

[Dr. MMX]

Its not enough informations to tell you something more. Its chemistry, so guessing is not in the place.
We only do know some details, but I could "bet" that you could exceed temp, pour acetone too fast, not ccorrect stirring, acid too fast

 

[cocojumbo]

everything is very well described here.

 

[Dr. MMX]

we dont know purity, temperatures of reagents
enivorement, temp in the room
values of time for reactions and temperature and conditions (like stirring) etc of reaction

Anything may be reason that this time it may be this "unlucky" time.

 

[Toddler]

@Dr. MMX

PLZ Can you explain acidification process with details.?
Today also i tried but aae result.


Also my other qus,

1. Chilled acetone means how much temp need?
2. Can i add in portions?( 50ml x 4time)
3. HCL add one drop after every 5 sec, before add i checked ph level?


Thank you in advance

 

[cocojumbo]

U can throw all acid and one time mix and this all ethyl acetate work the same like acetone

 

[cocojumbo]

the reaction with methylamine did not take place at all, as can be seen from the free base

 

[William D.]

For 20g, do the reaction without cooling, repeat the process. But when you acidify, use cooling.

 

[Toddler]

How much below temp,
I take reaction under 20°,
With use 1° ice water bath.

 

[William D.]

This should be enough. But you can reduce the temperature to 10*C.

 

[Toddler]

Ok I tried

 

[Toddler]

@William D. can you Elaborate details of acidification how i do fine.

I think i do some mistake in acidification.

 

[cocojumbo]

the reaction with methylamine did not take place at all, as can be seen from the free base. Is no problem throw acid xD is problem chemiclas and synthesis. You made somting what u dont Undersend

 

[cocojumbo]

This is How look like your freebase and is 1 way how can change freebase to yellow oil

 

[cocojumbo]

U use how the oil change

 

[cocojumbo]

And i do it one more time and get pure yellow
This is How need to look freebase

 

[cocojumbo]

Cold freebase and all acid in 1 time ph4