A little on the oxidation of benzoic aldehydes to benzoic acids via air
or at least a mention.
from the book
It was Wohler and Liebig that found that benzaldehyde oxidized in the air though it was
Carl Strange that Identified the crystals as the acid.
Sciencemadness thread on the formation of paraformaldehyde from formalin solution
http://www.sciencemadness.org/talk/viewthread.php?tid=19529
this used vacuum distillation to generate the paraformaldehyde
but if no vacuum is used the formalin can be distilled to make a clean solution of formalin
which I have done quite a few time from the fish medication
edit due to no triple post rule
with more searching it seems the best source of the triethyamine for the formylation
would be
Triclopyr Triethylamine Salt Cas 57213-69-1
a couple of examples of products with this in them are
TEA salt1.pdf (94.9 KB) TEA salt2.pdf (233.3 KB)
how to create our anhydrous magnesium chloride salt by going through ammonium magnesium chloride hexahydrate.
https://sci-hub.tw/https://doi.org/10.1016/j.apt.2010.01.003
Nitromethane in Polyphosphoric Acid A New Reagent for Carboxyamidation and Carboxylation of Activated Aromatic Compounds
Distilling Nitromethane from OTC RC car fuel (Go Kyosho Inferno all the way)
How to make PolyPhosphoric acid by heating hydroponics ph down.
http://www.sciencemadness.org/talk/viewthread.php?tid=69862
Typical Procedure: Preparation of Benzoic Acids 7a–d
Corresponding aromatic compound 1a–d (1 mmol) and nitromethane 2
(0.244 g, 4 mmol) in PPA (3–4 g) was stirred at 90–95 C for 5–8 h (Table 2). The
reaction mixture was poured in water (30 mL) with intense stirring and then cooled
to 0 C, and sodium nitrite (0.069 g, 1 mmol) was added. The reaction mixture was
stirred at this temperature for 15 min, and benzoic acids 7a–d were precipitated.
The resulting mixture was extracted by CH2Cl2 (1030mL). The solution was evaporated
under vacuum; the residue was purified by crystallization from water.
WOW!!!, that is a huge mark up. What a F*cken Ripeoff.
Wholesale pricing I have seen is between $11K -$15K per Kg.
carboxylation of resorcinols with methylmagnesium carbonate. synthesis of cannabinoid acids…pdf (127.5 KB)
probably not the best way to go but the first in history.
it should be noted that comercial methyl magnesium carbonate comes in normally either
DMF or methanol.
I would say they got the DMF one for the reaction so DMF may not be necessary (though
I may be wrong about that)
Having a little trouble understanding, they only got an 18% yield CBD → CBDa and only recovered 3% of the input CBD? I must be reading it wrong
I get the feeling its a small part of a total synthesis paper and has probably got rushed out
to get a few students on the title so they keep excepting lollys.
the real goods are probably in the profs hand worked total synth paper.
ill check and see but thats a guess without looking.
na that looks right
In a typical experiment cannabidiol (IIb)’ (314 mg.,
1 mmole) was heated at 120’ for 3 hr. with a 2~-solution
(1.5 ml) of MMC in dimethylformamide. After acidification
with dilute HC1, followed by ether extraction and purification
by preparative t.l.c., cannabidiolic acid (IIa) (300 mg.)
and cannabidiol (IIb) (8 mg.) were obtained.
though there is some loss there somewhere as CBDa is heavier than CBD.
8mg / 314mg is 0.025~ or 2.5%
I recall Elliot had a tech on his site that used high ass pH to make cannabinoids migrate to aqueous later, and left cbd etc in organic phase
Then used hcl or h2so4 To reacidify it
And it precipitated maybe as when it’s acidic it ain’t water soluble
This one using DCM?:
Not sure I do remember it was a/b and it may have been in scam but I thought halogenated hydrocarbons were a Nono
Depends on how confident you are that you can get rid of them all I guess
Regioselective Enzymatic Carboxylation of Phenols and Hydroxystyrene Derivatives
Regioselective Enzymatic Carboxylation.pdf (311.5 KB)
THE KOLBE-SCHMITT REACTION
THE KOLBE-SCHMITT REACTION.pdf (1.9 MB)
I think my first attempt will be with sodium ethyl carbonate in a steel threaded container/ pipe bomb
add some dry ice or butane so you get the 10 atm seal then heat too 185C for 7 hours.
if the results in the tables in the paper are anything to go by it should yield about 70%
we make the sodium ethyl carbonate from sodium ethoxide and then gassing it in a soda stream 
sodium ethoxide can be made from sodium hydroxide and ethanol.
Way to hot < 75 C is tops
thanx I am only going on whats in the paper at the moment and have not tried it.
they do the reaction in the microwave as well but the yields go down quite a lot.
will this reaction even happen at 75C ?
The chemistry of resorcinol carboxylation and its possible application to the CO2 removal from exhaust gases
Carboxylation of Phenols with CO2 Atmospheric Pressure.pdf (471.3 KB)
I think this is the paper that the gentleman above who sugested a test with bicarbonate and thc
was talking about.
Pressurized CO2 as a carboxylating agent for thebiocatalyticortho-carboxylation of resorcinol
Pressurized CO2as a carboxylating agent for thebiocatalyticortho-carboxylation of resorcinol.pdf (1.5 MB)
or it could be this paper he was on about.
The Carboxylation of Resorcinol and the Separation of beta and y-Resorcylic Acid by Ion-exchange Chromatography
I have a funny feeling that it will not work as it is above the decarb temp of THCa and is not
under CO2 pressure which I think turns the equalibrium in favor of carboxylation.
youtube of reaction with bicarb
so if we have a look at the first paper in this post the one titled blah blah CO2 removal of exhaust blah
blah
they get a doubling of yeild just by adding a carbon dioxide atmosphere.
I would put this down to the competing reaction of heat caused decarboxylation and
the carboxylation of the phenol with the bicarb.
though untested yet I would at a guess say that this would also be the case with THC
though the temperature of decarboxylation is lower than resorcylic acid.
hence the idea of using dry ice in a pipe bomb to increase pressure and push the reaction to the
right.
Another interesting paper
Kolbe–Schmitt type reaction under ambientconditions mediated by an organic base
Kolbe–Schmitt type reaction under ambientconditions mediated by an organic base.pdf (1.4 MB)
this one is done at 30C and has reference to THCa though not directly they are hinting at its
usability for it I think.
they are getting quantative yeilds from an organic base guanadine with the resorcinol
in acetonitrile under 200 ATM of CO2
There are two other whom have this sent to them as I’m having it “dummy proofed” essentially. But for now here’s a rough write up that’ll point y’all in the direction you’re headed to. I’ve done this on small scale, it works, but only changed solvent from etho - heptane, better choice of the two for it. ( the e6ho was a mishap but showed me r&d on the concept of this procedure. I’m Workin on making this easy to understand & make some more sense of some of the steps but like I said here it is for now as a draft. This is able to work d9 as well. If any questions feel free
