Method 1. Acetic Acid 10VOL solution with bark 100g, soaking and stirring for 3 days. 2. Sodium hydroxide 100g to ph 12. 3. Warm for 20 mins at 35 celcius. 4. DCM pull while stirring/heating at 35c. 5. DCM isolated for xtalisation. 6. Acetone added. 7. Freeze precipited on stirrer.
Question Can Heptane be mixed with (step 5) DCM solution, mixed, (possibly heated + stirred to emulsion and then de-emulsioned) and heptane then pulled, to precip extract some white crystal? If so , SWIM would like to order some heptane to a supplier which SWIM has found for a cheap price ($20 /liter)
SWIM received molasses from his last DCM xt, enjoying fast but true breakthrough, but wants to continue, with isolating, choping and changing, etc.
Thank you for reply, sorry about my English! Many thanks
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1. Acetic Acid 10VOL solution with bark 100g, soaking and stirring for 3 days.
This is fine.
2. Sodium hydroxide 100g to ph 12.
This too.
3. Warm for 20 mins at 35 celcius.
Don't bother with this bit.
4. DCM pull while stirring/heating at 35c.
Don't heat as DCM is more than powerful enough to pull all the goods as is. Heating will just pull excess crap. Also I wouldn't heat DCM as it will boil a little over room temperature.
5. DCM isolated for xtalisation.
All you can do with DCM is evap it or maybe salt out. 6. Acetone added.
Why?
7. Freeze precipited on stirrer.
Out of what? You can't freeze precip out of either acetone or DCM.
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