THC Removal From High CBD Strains Decarboxylation

nebor

New Member
I was reading some old posts with some errors in information but one of them caught my eye. I have recently wanted to eliminate the THC component of my CBD oil without having to take it to Isolate or using chromatography or even fractionation to do this.

The older post suggested that THC-A will decarb to CBN faster then from THC-A to THC and thus it would be possible to turn the THC component into CBN eliminating it from the CBD oil. Because decarbing THC happens at lower temps and times is this possible? Is there a particular heat/duration to maximize this?

Personally I have never experienced this. When decarbing CBD-A to CBD in the past, if we went "OVER" or decarbed for too long or at too high a temp, the THC did not seem to be affected and in most cases was higher than starting. Any insight into the possibility of using decarboxylation to "remove" THC from CBD oil (or in this case convert to CBN).?

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In my experience you can not eliminate it either. But you can start with a variety, which has very little thc-a and as much cbd-a as possible. I decarb it for one hour at 120-130*C. I do not have a possibility to analyse, this is what I have read.
 
You would have to use fraction distillation or long column chromatography. That would be the best way to isolate CBD. The problem is that The boiling points are very, very close. THC's boiling point is 157°C while CBD boiling point is 160°C. The boiling points are so close that it would be very hard to separate them using fraction distillation but it would be possible. Long column chromatography on the other hand would isolate it much easier.


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You would have to use fraction distillation or long column chromatography. That would be the best way to isolate CBD. The problem is that The boiling points are very, very close. THC's boiling point is 157°C while CBD boiling point is 160°C. The boiling points are so close that it would be very hard to separate them using fraction distillation but it would be possible. Long column chromatography on the other hand would isolate it much easier.


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Yes.. I have tried fractional distillation... it is not happy. Column chromatography is no problem for me BUT.. the consumables and the time are more than I want. I know there is SOMEONE out there with a process that is cheap because they are selling their THC removed oil for the same price as the oil with natural levels of CBD.
 
The silica is cheap enough and reusable. I would probably recommend chloroform for the Mobil phase. You can synthesize it very cheaply from bleach and acetone. The column and valve is probably the most expensive part. A good column runs about $200.


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I wouldn't worry too much about THC isolation/removal. If you want a higher CBD ratio try using industrial hemp. It's very high in CBD and very low in THC.


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Here's the Adams patent from 1940 describing the method of CBD isolation.
"It has been found that from the extracts of hemp (Cannabis sativa or Cannabis indicia) a red viscous oil can be obtained, commonly known as red oil, from which a pure crystalline compound, cannabidiol, can be isolated (Adams, Hunt and Clark, J. A. C. S. 62, 196 (1940). Through a chemical study (J. A. C. S. 62, 196, 732, 735, 1770 (1940); see also J. A. C. S. August and September numbers, 1940), it has been shown to have the structural formula: CH3 OH C OH CH3 CH2 (Formula I)

With the exception of the position of the double 20 bond in the left hand cycle in the above formula the structure of cannabidiol is well established. Investigations show this left hand cycle to be a tetrahydro benzene ring.

Cannabidiol is a crystalline compound, M. P. 66-67° (cor.), and forms long white rods when crystallized from petroleum ether (B. P. 30-60° ). It has an [a]27D-125°, and is physiologically inactive so far as marihuana activity is concerned.

The principal object of the present invention is to provide an improved process for isolating cannabidiol from red oil obtained from hemp.

Other objects of the present invention will be apparent as the description proceeds.

The isolation of cannabidiol from red oil obtained from hemp is described in detail in J. A. C. S. 62, 196 (1940). This process which includes the treatment of purified red oil with 3,5-dinitrobenzoyl chloride and the formation of cannabidiol o, bis-3,5-dinitrobenzoate has been found of particular value for the isolation of the desired product. Ammonolysis of the benzoate, i. e. diester, yields cannabidiol in pure form.

The process as set forth in the J. A. C. S. 62, 55 196, 198, 199 (1940) serves to illustrate the present invention.

Cannabidiol bis-3,5-dinitrobenzoate.-A solution of about 50 grams of purified red oil, B. P. 175-195° C. (2 mm.), in 200 cc. of dry pyridine was poured rapidly with shaking and cooling on 85 grams of 3,5-dinitrobenzoyl chloride. The mixture was heated on a steam cone for two hours with occasional shaking and was then poured into ice and hydrochloric acid (200 cc. of concentrated hydrchloric acid, 500 cc. of ice). It was filtered or decanted and the insoluble material was washed several times with dilute hydrochloric acid. The residue was dissolved in 600 cc. of benzene and filtered. The insoluble material consisted mainly of 3,5-dinitrobenzoic acid.

The benzene solution was washed with dilute hydrochloric acid, then with aqueous sodium bicarbonate and finally with water. The benzene was evaporated and the residue was dissolved in 500 cc. of dry ether. This solution was treated with norit (20 grams), filtered, and then concentrated to 300 cc. On cooling in an ice-salt mixture with constant stirring, crystallization set Sin. After one hour, the product was filtered and washed with cold dry ether. Upon purification of the desired product by recrystallization from 800 cc. of a mixture of methanol and methyl acetate (2:1), it was obtained as white rods M. P. 106-107° C. (corr.).

Cannabidiol.-A solution of 50 grams of cannabidiol bis-3,5-dinitrobenzoate in 100 cc. of toluene was placed in the glass liner of a high pressure reaction vessel. The mixture was cooled by dry ice and about 100 cc. of liquid ammonia passed into it. The liner was then placed in the high pressure reaction vessel and the cover quickly fastened. The high pressure reaction vessel was allowed to stand for five hours at room temperature. At the end of that time the excess ammonia was allowed to escape and the product, which had set to a solid mass, was digested with 400 cc. of petroleum ether (B. P. 60-110° C.). The solid 3,5dinitrobenzamide was filtered and washed with two 50 cc. portions of petroleum ether. Filtrate and washings were combined and extracted six times with 150 cc. portions of boiling water to remove the last traces of 3,5-dinitrobenzamide. The petroleum ether was then evaporated and the i residue distilled, B. P. 187-190° C. (2 mm.) (bath temperature 220° C.). The resulting product, i.e. cannabidiol, was obtained as a pale yellow resin.[/b]

It will be obvious to those skilled in the art that the present invention is not limited to the details of the process outlined above. The scope of the present invention accordingly should be determined by the claims annexed hereto.

1. In a process for isolating cannabidiol from red oil obtained from hemp, the step which consists in treating the red oil with 3,5-dinitrobenzoyl chloride to form cannabidiol bis-3,5-dinitrobenzoate.

2. In a process for isolating cannabidiol from red oil obtained from hemp, the step which consists in isolating the cannabidiol from said oil as the dinitrobenzoate ester.

3. A process for isolating substantially pure cannabidiol from red oil obtained from hemp which comprises (a) treating hemp red oil with 3,5-dinitrobenzoyl chloride, (b) separating the cannabidiol bis-3,5-dinitrobenzoate formed in (a) from the red oil mixture, and (c) subjecting the benzoate ester of (b) to ammonolysis.

4. The product cannabidiol bis-3,5-dinitrobenzoate.

ROGER ADAMS.

Written August 16, 1940"


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The silica is cheap enough and reusable. I would probably recommend chloroform for the Mobil phase. You can synthesize it very cheaply from bleach and acetone. The column and valve is probably the most expensive part. A good column runs about $200.


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Chloroform works great on THC but a little less so on CBD at least as I have found. Maybe I need to start packing my own columns but I think I am missing some chemistry. I am pretty sure that the big dogs have moved on from chromatography to strip the THC. It has to be a wash or be happening during primary extraction. I have heard whispers that you can modify a SCFE machine to just pull CBD. All the material I am running is already industrial hemp up to 60:1 ratio but I am still getting my good oil too "HOT" for export. Any traceable amount of THC is not acceptable for some of my destinations. But the customers want oil as opposed to Isolate and other guys are able to do it. Just haven't figured it out yet.

You mentioned using chloroform as the mobile but doesn't that also rip up (add to) the cost??

I have seen that old patent you pulled up. It's a BEAR to do ... I would stick with silica before Breaking Bad with that damn patent LOL
 
Chloroform works great on THC but a little less so on CBD at least as I have found. Maybe I need to start packing my own columns but I think I am missing some chemistry. I am pretty sure that the big dogs have moved on from chromatography to strip the THC. It has to be a wash or be happening during primary extraction. I have heard whispers that you can modify a SCFE machine to just pull CBD. All the material I am running is already industrial hemp up to 60:1 ratio but I am still getting my good oil too "HOT" for export. Any traceable amount of THC is not acceptable for some of my destinations. But the customers want oil as opposed to Isolate and other guys are able to do it. Just haven't figured it out yet.

You mentioned using chloroform as the mobile but doesn't that also rip up (add to) the cost??

I have seen that old patent you pulled up. It's a BEAR to do ... I would stick with silica before Breaking Bad with that damn patent LOL

I synthesize my own for about $12 a gallon.
Bleach/acetone at below 0°C->exothermic reaction then decant off the aqueous layer (or use a sep) and distill the chloroform via SPD. If you don't distill, any residual acetone will form an azeotrope and contaminate your trichloromethane.
The only serious problem with chloroform is that it's carcinogenic so the final product has to be be oven vac'd. And I recapture my used chloroform in a closed loop cold condenser.


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