amination process failure keeping temp

[nimrod313]

Hello fellows

Yesterday tried for first time make a big batch 3.5kg 2b4m...
At amination process adding methylamine hcl to the dcm with 2b4m I couldn't handle temp and it rinse to 55⁰ and dcm boiled because of it...
Eventually after first layer saperation at start of wash when I added distilled water it mixed with freebase and not saperate
I mixed all saperate freebase for 40 min and it became light blue color
Any ideas or methods to extract the freebase and save it or it dead?

 

[loadingST]

Once i made similar mistake by closing the flask while the temp inside rose so muxh and when i open the cap the whole aolution of lachymators and amines went on my face xd cathinones chemistry is colorfull, i have made some ketones by myself and have had green colors but never blue espesialy at the crystalization proces, ao if i understand core tly you have extracted it into plain water acidic water and when it reacted qith the avid the whole thing become blue ? Get the water layer whatever color is it, dry it, and recrystalize the product to purify from these colorfull byproducts.

 

[nimrod313]

Its all because I went on large scale without proper cooling... the dcm boiled of exothermic effect of the NaOH react with methylamine hcl
I preform after that the process with EA and cooling bath
Now waiting for yield results
Experienced before with EA but yield was a bit lower than with dcm now want compare again

 

[loadingST]

You shoud have just prepare a cooled NaOH aolution, and add slowly to prevent this.