P Toluenesulfonic Acid

(All done at room temp while in the reactor)
-Put 10kg’s of CBD isolate in a glass reactor.
-Add equal parts of heptane to reactor. (1:1)
-Slowly stir the solution while the heptane fully dissolves the CBD creating a homogeneous solution.
-Add 1% p-tsa
-Ramp up the rotations on the reactor.
-Smoke a joint and go to bed.

Washes:
-(x1)Add equal parts of distilled water to the Δ⁸ solution in the reactor (1:1), lightly stir for 5 mins, then let sit and separate for 30 mins, discard distilled water+gunk.
-(x2)Add equal parts BiCarb solution to the Δ⁸ solution in the reactor, lightly stir for 5 mins, let sit and separate for 15 mins, discard BiCarb+gunk.
-(x2)Add equal parts Brine solution to the Δ⁸ solution in the reactor, lightly stir for 5 mins, let sit and separate for 15 mins, discard Brine+gunk.
-(x1)Do another distilled water wash and discard water+gunk.
-Collect the cleaned up Δ⁸ solution into 5gal buckets.

Then…
-Roto down the Δ⁸ solution to a viscous Δ⁸ crude.

Then…
-Add Δ⁸ crude to a SPD.
-Add a “pinch” of carbon into the boiling flask.
-Distill Δ⁸ crude into Δ⁸ distillate.


The CBD fraction of column chromatography can be distilled (bp 187-190° C/2 mm; pale yellow resin) to purify it. Isomerization can be accomplished with any of several solvents and acids. Alcohol and sulfuric acid isomerizes only 50-60% of CBD to THC; p-TolueneSulfonic Acid (p-TSA) in petroleum ether or other light, non-polar solvent will convert 90% of CBD to THC upon refluxing 1 hour at 130° F. (16, 17)

Reflux 3 gr CBD in 100 ml dry benzene for 2 hours with 200 mg p-TSA monohydrate until the alkaline Beam test (5% KOH in ethanol) is negative (no color). The Beam test gives a deep violet color with CBD. Separate the upper layer, wash it with 5% sodium bicarbonate, wash again with water, and strip the solvent. The remaining viscous oil should give a negative reaction to the Beam test. The crude THC can be purified by distillation (bp 169-172° C/0.03 mm), or by chromatography in 25 ml pentane on 300 gr alumina. Elute with pentane 95:5 ether to yield fraction of CBD and THC. Combine the THC fractions and distill (bp 175-178° C/1 mm).

Reflux 2 gr CBD in 35 ml cyclohexane, and slowly add a few drops of sulfuric acid. Continue to reflux until the Beam test is negative. Separate the sulfuric acid from the reaction mixture. Wash the solution twice with aqueous sodium bicarbonate, the twice again with water. Purify by chromatography, or distill (bp 165° C/0.01 mm). Any unreacted CBD can be recycled.

Another method is to reflux a mixture of 6 gr dry pyridine hydrochloride and 3 gr CBD at 125° C until the Beam test is negative. Wash the reaction mixture with water to remove the pyridine, then extract the mixture with ether. Wash the ether with water, evaporate the ether, and distill the residue i.v. to yield pure THC.

Similarly, reflux 3 gr CBD in 150 ml ethanol with 50 ml 85% phosphoric acid until the Beam test is negative. Work up the reaction mixture, and purify the THC.

Alternatively, reflux 3 gr CBD in 100 ml absolute ethanol containing 0.05% HCl for 19 hours. Extract the ether, wash the ether with water, dry, evaporate, and chromatograph on 400 gr alumina to yield:

(a) 0.5 gr 1-EthoxyHexaHydro-CBN (EHH-CBN: mp 86-87° C); elute with pentane 98:2 ether. Recrystalize from methanol and water.

(b) 2 gr THC; elute with pentane 95:5 ether. Repeated chromatography will separate the less polar forms.

(c) 0.5 gr EHH-CBN, eluted with pentane 93:7 ether. It can be isomerized to THC by refluxing in benzene for 2 hours. Cool the reaction mixture, wash it with water; separate, dry, and strip the solvent layer i.v. to yield THC.

CBD also can be isomerized by irradiation of a cyclohexane solution in a quartz vessel with a mercury lamp (235-265 nm) for 20 minutes. Workup of the reaction mixture yields 7-13% THC. (18-20)

—-

With one set of equipment. 100L Reactor, 50L sep funnel, 50L rotary evaporator and one 20L SPD we can crank out 13kg every 4 hours or so.
Screenshot_20200317-185900_Drive
Screenshot_20200317-185900_Drive1080×2220 421 KB

Reaction starts with 13kg of CBD isolate as that is the maximum amount of isomerized product that can be comfortably held in the boiling flask of the 50L rotary evaporator.

Reaction is performed in the 100L reactor.

13kg CBD isolate is dissolved into methanol or ethanol.

Solution is heated in reactor to 63C.

300g of catalyst is added (P-TSA

Reaction is allowed to carry on for 47m to achieve the results in the attached COA.

Solution is then drained into buckets. Filling 1/3 of each bucket. 15 buckets total.

Buckets are then filled to 2/3 level with organic solvent (hexane/heptane)

Buckets are then filled to the top with water to elute the cannabinoid solution and separate into an aqueous/organic separation. Catalyst is dissociated into the water alcohol mix while the cannabinoids go with the organic solvent.

The mix is then poured into the multiple 50 or 100L sep funnels and separated…

Dispose of aqueous layer. Retain organic layer for solvent recovery.

Feed organic solvent solution through rotary evaporator and recover all solvent. Bath temp starts at 40C and is raised as high as 90C once most organic solvent is recovered. Diaphragm vacuum pump is then switched out to a 2 stage rotary vane to achieve a deeper vacuum and remove Max amount of solvent.

Cannabinoid mix is then poured into 20L SPD and distilled to remove any remaining solvents and byproducts (p-cymene)

Reaction time can be decreased to achieve more ?9 or increased to make all ?8.

Bam THC distillate on the cheap.

I hope this information serves all well and helps make the consumption of THC for medical and recreational purposes more affordable and available for everyone. CBD is legal to ship throughout the US and most parts of the globe. THC will no longer need to be shipped across borders.

Also I hope that this information brings about or helps push through the global legalization of marijuana.

It costs $300-$500 to make one pound of 92% THC distillate. Let’s bring the price of that 25% THC flower down to $125/lb =P

If anyone appreciates this posting buy your CBD isolate and equipment through me. I can also come in as a consultant to assist in the development of labs of scale for minimal cost.

Unless otherwise stated, the content of this page is licensed under Creative Commons Attribution-ShareAlike 3.0 License