Jag försöker 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

 

[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.

 

[Toddler]

Ptfe stirrer rod or stainless steel rod

 

[dodobird]

In the initial stages no visible nice layer of the freebase is visible, right?

 

[dodobird]

Don't laugh but I saw this on somewhere that color not showing any meph likee it should after adding ma40 and allowing to settle the layers... might need gentle heating within 50 to 55 dg regulated for 30 minutes or more perhaps an hour ..so the oil forms nice rich deep color deep yellow seems the best from what i read but most people get brown depending on the bk4 acquired and other reagent quality. Then washed 3 x put in freezer/fridge for an hour before acidified to 5.5 dropwise .. what say you?

 

[dodobird]

What did your 2b4m look like ...can u share a pic, please?

 

[William D.]

EA with aq. methylamine becomes almost homogeneous when stirring. This is the main reason for a quick reaction. If there are problems with separation, you can use heating, brine or additional EA.

 

[Toddler]

@William D.
EA with aq. methylamine becomes almost homogeneous when stirring.

How much temp range ?

 

[dodobird]

Was talking to the original poster but since u replied, care to share a pic?

 

[dodobird]

Meph and or ma40 likely culprit, his 2b4m don't look that good afaik