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Why remove water from freebase? When you drip 37%hci while acidificaction, you still have water inside again. It makes no sense at all. And by the way, after acidificaction i take the water layer and dispose the organic layer. Water layer is placed in several bowls to evaporate, after a few...

Do you acidificaction with acetone dilluted hci? I think the red color blames to acetone. Try 37%hci (icecold) without acetone, use icecold dest water mixed with freebase and prepare dest water icecubes. While acidificaction the rm becomes warm and with icecubes you can bring temp down. Or use...

Crush it to powder, wash with icecold acetone, then recrystalisation with dest water/ipa , dest water/acetone or just Methanol (5ml per 1g Powder). Some use only water but this takes more time to evaporate

After acidification you have to separate the organic from water layer and put the water layer in some dishes/containers and let them stand for some days, sometimes +1 week, depends on volume. Crystals begin to form when 50% have evaporated. When crystals have stopped forming and they are not...

E ethylacetate, short reaction time

E ethylacetate

Reaction time is mentioned in my text. Depends on solvent. But the whole process(with acidification ,etc) can be done in 4-5 hours (DCM) or 2 hours (ethylacetate). Icecold acetone is used to remove some impurities, that is called washing. Works with buchner filter+Vakuum pump and also with...

You better buy some bmk (CAS 5449-12-7) from China, then hydrolysis via one of these acids. https://chemlabsupplies.co.za/product/phosphoric-acid-85-fg/ https://chemlabsupplies.co.za/product/hydrochloric-acid-32-*****/ https://chemlabsupplies.co.za/?s=Acid&post_type=product&dgwt_wcas=1

Crush the crystals to powder with mixer, wash then, recrystallisation

Why do you want to do this? I see no sense in it, you cant evaporate freebase and expect that crystals will form...you can put it into freezer but the results are not the same as with water

Could you give me an advice, how you do it?

Yes, heat until 36 degrees 300ml per 100g 2b3c

Even with DCM i only got 40% yield...

How do you get this result?

Not very much, 30-40% max.

No temp control needed, just mix and stir for 20min... temp rises and falls from the reaction itself

I had also results with acidification in freebase only but were not as good as with water together and evaporate the water layer. Recrystallisation after acidification should be possible but if the crystals are cleaner then, i can not say.

It does not fall out while acidification... The crystals form while evaporation from the water layer.

There are different methods listed in the forum, just look for it.

So, when you have your real contacts, start your doing your business with them, not with anyone from here. Nodody knows you and it seems, that even nobody tries to accept your offer.