Question need a help here a little.

[elpatron7]

Hi ola friends,

I'm new to this I'll be straight on point.
I had 250gs of pure 2b4m straight from
international. I mixed 500ml of benzene in a 1 litre glas flask. And
350ml of 40% aqueous solution (all good 99.9% lab grade) following all steps for this mentioned in the simplest one. Then I stirrered it periodically for 24
hours. 2 layers where formed bottom was navy blue and top was like dark honey. Then I transferred it to a plastic 2 litre bottle flushed it with a little warm water 38•c
water properly. And drained it kept the top layer and used 1/10 36%
concentrated hcl 150ml 900ml-1litre of acetone and used a pipette to transfer
it for acidification. (Took small portions in a 2litre beaker. Waited as the fumes started to roll.. nothing
happened after 2 mins so I rolled up all acetone concentrated hcl mix
altogether into it after doing it for 35-40 times. Now 2 layers r
formed. One which seems thick is on the bottom and on the top is dark
brown cold chilled liquid I feel acetone. I don't know what went wrong I
wanted to synthesis 4mmc all the materials used are 100% lab tested and
procured from original sources. Now I have left with a 2000ml of
liquid brownish dark black. What to do help. ?
And please help me with what went wrong.

 

[Dr. MMX]

Hello.
Lets focus about your start of the synthesis to have a clear view on the case.
So you put 250g of 2b4mp into 500 ml of benzene did it dissolve in it?. 350 ml of methylamine aq was added. Was bottle closed or open afgter you added methylamine 40%aq?
What temperature was in the place you beggined this steps?

 

[elpatron7]

Temperature was room 33-35°c yes 2b dissolved only minor particles stayed undissolved. Then aqueous solution was added n cellophane sheet and tape around the neck it was stirrered for alternate hours.

 

[Dr. MMX]

I think you should wash it with cold water (after reaction). If you added once little amount of water at 38c it could not wash the methylamine properly. I think you used too little of the solvent as well, if you decided to do that I think some extraction should be performed before acidification.
I do wonder how pressure didnt build there if you used 1l bottle while using 80-90% of it. I dont know what kind of bottle you had but I think it could explode (depending how you added methylamine etc)

How did you add methylamine? what was temperature after you added it?