well BP ethyl-acetate…is 77 C. Maybe 35-40 C. and then evaporate…slowly for a week or two open glass dish? or rotovap…if you have one…
a vacuum oven if you have one.???
Keep out of the light…dark room…and be patient…
You could try saturating the ethylacetate with water first as a different experiment.
But if you get such nice crystals with ether…why change?
Ether, is not such a bad solvent, people in Ireland drink it. I do not think
it is as toxic as Ethanol. A little ether left over…is nothing.
I have tried Ascorbate…now I need to try Ascorbic.
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Yeaa i know that ether is not so bad, maybe S Thompson can tell us haha.
I have all of that.
Maybe in a Duran Laboratory bottle* or close vessel with sugar and ethylacet then heat until practical all sugar dissolve and then ramp down?..
… i am trying to figurate a rapid crystalization like some people can
Edit* or ethanol maybe can archive this ramp down metod, is no so volatile. And little descarboxilation dont hurt …
I dont have the biomass to try all this now… but i am on this.
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This old chemist says
Ethyl acetate just for
Chromatography
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Sorry if i bother with the question, i love to learn, can you tell me why only for chroma?
Thanks
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Ethyl acetate has a functional group that may or may not take part in reactions, especially when heated and with other functional groups present.
But great for adjusting polarity of hydrocarbons.
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Can you give an example of the ester reacting with any thing
other than water? Curious. …ones that you are concerned about?
Check out USDA list of chemicals approved for “certified organic”
food preparaion. The list is very short.
If were are making a Cannabinoic acid, we are limited to about 30C.
Personally I do not care for the smell. But as far a immiscible solvents with aqueous
the list is very very short. Other than the caveat, of “certified organic food prep”
I think there are scores of better solvents. Including ether which is a rather non
toxic “intoxicant” when compared to alcohol. Hexane is notably toxic.
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In principle, any ester can undergo trans-esterification with any alcohol given sufficient nucleophilicity, high enough energy input, and “pH”.
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that might explain a few things. ! especially at pH 11-13.
good point…
do you have a specific example in the world of cannabinoid chemistry?
If you were to precipitate aqueous cannabinoate at pH 13 (0.1N NaOH)
with 5% HCl @ pH 2…then back extract with ethylacetate would you expect some
problems?
I may have tried ethylacetate scrub at pH 13 and noticed some odd things after
drying and Chromatography…I can not remember specifics…sometime ago.
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Since you mention the subject i always ask me some things in this matter. After the extraction with NaOH 0,1 N water, the reamainin organic phase with the terps are useless? Or can be washed with acidic water to neutraliz purific and use in future. There are so bad the yields in this procces? When i was doing this, after evap the pentane of the thca phase it looks like destilate, very clean and hard, and the remainin organic phase whit the terps(cloudy) when evaporate smell pretty well.
edit, i remember when i precipitat with HCI theire form an abundant offwhite mass of thca, maybe was to much hcl but…was beautyfull that mass (to me with naked eyes not wass too bad the yields)
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If you do it, make sure you shake well, then repeat.
there is a lot of “color” left in organic phase…
I dont really know what is left. The THCA should be in Aqueous.
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So we dont know whats happen to the terps, always i ask me this, if is viable and profitable purific separately. Destil or remediate terps and then recombine with the thca crystalizated.
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thanks for the replys and you amiability
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Sorry , the terps! It all depends on what your first step is: fresh, fresh frozen, dried
and or predecarboylated…and strain…to begin.
Each first step solvent will be different.
But if you just what we are talking about here…what ever terps you have
left probably stay in the organic phase when extracting into pH 13 H2O.
The water process for THCA simply produces a clean (to some extent)
product, amorphic crystals…when vaped…people say it is kick ass hyper speedy,
but no one likes the taste. It doesn’t produce a product that relates to your past taste
experience with marijuana products. Why would it ? Its a water processed product.
So to answer your question: The terps are gone… Yes, I think people may market products that have terps reintroduced.
BTW…I havn’t got to the Ascorbic acid yet…
best regards,
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It is truly a delight to see so many brilliant chemists chatting here! And yes, @Vegeta , you ARE a chemist! You have some very keen insights that take you out of the category of “layman” when it comes to chemistry, so I believe you have the soul of a chemist, even without institutional education in the subject.
To answer your question, there should NOT be anything hazardous in the product after having done what you described. Therefore, I would recommend to taste the product, about which I believe @mitokid asked you. In this case, “TASTING” means licking the solid product with your moist tongue… not necessarily vaporizing and inhaling it to “taste” the vapor.
To determine whether or not it contains any residual ascorbic acid (which I believe it may), you “will do some tasty test” 
with just a tiny chunk (maybe the size of 1-4 crystals/grains of table salt or sugar) to look for SOUR FLAVOR. Sour flavor means there is something acidic present. To be more certain the sourness you may taste in your product is actually the ascorbic acid you added, you may also taste an equally tiny amount of the pure ascorbic acid.
If your product DOES contain (tastably “too much”) ascorbic acid, you will need a few supplies to clean it up, properly. Here is the procedure I ALWAYS recommend to achieve the perfect pH for cannabinoid products that have been treated with acid or base at some point in processing…
MATERIALS:
• product dissolved in alkane or similarly hydrophobic, aprotic solvent
• pure distilled water… Fyi, Reverse Osmosis [RO] filtered water is usually not good enough, so purchase jugs of distilled water or just make your own in a clean rotovap!
• pH litmus paper, full range or designed for pH 5-9
Or
• calibrated digital pH meter
PROCEDURE:
1. Measure & record pH of pure distilled water (straight out of the jug). It should be 6.2-6.8 pH at typical room temperatures.
2. Wash the non-polar solution of cannabinoid with 1/3rd its volume of that pure water… mix the liquids to emulsion perhaps 7 minutes.
3. Allow complete partitioning of the liquid layers. If the lower layer is the aqueous, drain a decent sample of it into a clean & dry glass vessel, without any emulsion (mid-layer “scum”) on its surface. If the upper layer is aqueous, it may be sampled as-is, without separation draining.
4. Now, measure & record the pH of this water again.
The difference between the pure water pH (step 1) and the post-wash water pH (step 4) tells you how close you are to the equilibrium pH…
(A)cid ~ If the previous wash used acid (e.g. citric or ascorbic), and wash pH is at or further than -0.3 BELOW (i.e: more acidic than) the pure pH, simply wash again with another 1/3rd volume of pure water, and measure post-wash pH again.
Repeat until wash pH is within -0.2 of or at pure water pH.
(B)ase ~ If the previous wash used alkali (i.e. a base like sodium bicarbonate), and wash pH is at or more than +0.3 ABOVE (i.e: more alkaline than) pure pH, simply wash again with another 1/3rd volume of pure water, and measure post-wash pH again.Repeat until wash pH is within +0.2 of or at pure water pH.
(C)orrect ~ If wash pH is within +/-0.2 of pure pH, it is acceptable. Ideally, the post-wash pH should be EQUAL to the pure water pH.
It is better to reach a “water equilibrium pH” this way than it is to bounce back and forth between washes with acid & base (aka: “titration”). Perfect titration of acid with base or vice-versa is nearly impossible without some means of continuously monitoring the pH, such as a colored indicator or a benchtop digital pH probe in the solution.
Best of luck, and thanks for sharing this! 
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This is why I brought up acetonitrile. In the case the crystalline material DOES taste like as if it contains ascorbic acid.
Sometimes in preparative organic synthesis, you encounter situations in which there’s this one special solvent that just too damn well suits the problem at hand and becomes hard to disregard.
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Thank to you very much for your suchs inspiring words…really apreciate in this moment. I am bulding my own little lab step by step for organic extraction and formulations of phytomediciness mixing concepts of all cultures and times. And i will work with academic people for the analisis and to give me green ligth of the formulas.
Thanks a lot 
Love💟
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Yes after the water extraction and precipitation of THCa no terps. My real question is if the terps that left in the first step and remainin in the organic phase there are broken or useless after “wash” with the PH 13 water.
Thanks
Bombastic thing developing here…
Dont stop there…
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And for CBDa this benefit still be the same, no?
If the addition of ascorbic acid truly promotes precipitation of THCa, I cannot see why it also wouldn’t be beneficial in the case of CBDa.
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