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The Not So Solventless Clear Concentrate From Harborside!
- Thread starter UNREGISTRD
- Start date
100% truth.
Daub Marley
Member
Exactly. So.... now who believes it is distillation still?
primeform
Active member
Is that a confession?
primeform
Active member
Seems this is all we need to do for pure THC..
Isolation of pure cannabidiol
If completely clear THC (a clear, thin, colorless oil) is desired, it is necessary first to isolate pure cannabidiol from the chromatographed oil by converting it to cannabidiol-bis-3,5-dinitrobenzoate. This is then converted back into pure cannabidiol, which is now in the form of white crystalline prisms. The process for this operation is found on pages 456 and 457 of the Lloydia
volume previously mentioned, and a description of it follows.
Cannabidiol-bis-3,5-dinitrobenzoate is made by rapidly adding 300 gm fresh 3,5- dinitrobenzoyl chloride (m.p. 68—69°C) to a
mechanically stirred solution of a chromatographed hashish extract in dry pyridine at 0° under nitrogen. The mixture was stirred for 15 minutes, then warmed in a 60°C hot water bath for 30 minutes. This mixture was then poured into a mixture of 200 gm of ice and 300 ml concentrated hydrochloric acid and extracted with ethyl acetate (750 ml). The precipitate was filtered and washed with another 750 ml ethyl acetate. The aqueous phase was separated and washed with 500 ml ethyl acetate. The combined organic phases were washed with aqueous sodium bicarbonate (2 x 200 ml) followed by 300 ml distilled water and dried over CaSO4. The solvent was removed in vacuum to yield 340 gm of a dark oil. This was purified by crystallization from 1800 ml ethyl ether, yielding 194 gm of off-white powdered cannabidiol-bis-3,5-dinitrobenzoate melting at 97—101°C.
Pure cannabidiol is made by adding 220 ml of liquid ammonia to a solution of 288 gm cannabidiol-bis-3,5dinitrobenzoate in anhydrous toluene (400 ml) at -70°C in a Parr bomb. The sealed apparatus was mechanically stirred. During five hours the pressure built to 110 psi and the temperature rose to 20°C. The ammonia fumes were released overnight. The product was dissolved in heptane (400 ml) and insoluble 3,5-dinitrobenzamide was removed by filtration. The precipate was washed twice with 150 ml heptane. The heptane solutions were combined and washed with boiling water (5 x 200 ml) and the solvent removed in vacuum to yield 120 gm of a dark oil. Chromatography on 180 gm of this product on 3400 gm of Florisil and elution with 30% chloroform in hexane yielded oily cannabidiol (140 gm).
Crystallization from 30—60° petroleum ether yielded 99.2 gm white prisms, and
recrystallization gave 94.8 gm pure cannabidiol.
Conversion of Pure Cannabidiol to Pure THC
The crystalline prisms of cannabidiol are converted to pure THC utilizing a formula of Roger Adams found on page 2211 of volume 63 of the Journal of the American Chemistry Society. The following is a description of a method for producing pure THC.
Isomerizing the cannabidiol with sulfuric acid
One drop of 100% sulfuric acid was added to a mixture of 1.94 gm crystalline cannabidiol in 35 cc cyclohexane. After refluxing for one hour, the alkaline beam test was negative. The solution was
decanted from the sulfuric acid, then was washed twice with aqueous 5% bicarbonate solution and twice with water. It was then evaporated. This residue was distilled under reduced pressure to yield pure THC with a rotation range of 259° to 269°.
Isolation of pure cannabidiol
If completely clear THC (a clear, thin, colorless oil) is desired, it is necessary first to isolate pure cannabidiol from the chromatographed oil by converting it to cannabidiol-bis-3,5-dinitrobenzoate. This is then converted back into pure cannabidiol, which is now in the form of white crystalline prisms. The process for this operation is found on pages 456 and 457 of the Lloydia
volume previously mentioned, and a description of it follows.
Cannabidiol-bis-3,5-dinitrobenzoate is made by rapidly adding 300 gm fresh 3,5- dinitrobenzoyl chloride (m.p. 68—69°C) to a
mechanically stirred solution of a chromatographed hashish extract in dry pyridine at 0° under nitrogen. The mixture was stirred for 15 minutes, then warmed in a 60°C hot water bath for 30 minutes. This mixture was then poured into a mixture of 200 gm of ice and 300 ml concentrated hydrochloric acid and extracted with ethyl acetate (750 ml). The precipitate was filtered and washed with another 750 ml ethyl acetate. The aqueous phase was separated and washed with 500 ml ethyl acetate. The combined organic phases were washed with aqueous sodium bicarbonate (2 x 200 ml) followed by 300 ml distilled water and dried over CaSO4. The solvent was removed in vacuum to yield 340 gm of a dark oil. This was purified by crystallization from 1800 ml ethyl ether, yielding 194 gm of off-white powdered cannabidiol-bis-3,5-dinitrobenzoate melting at 97—101°C.
Pure cannabidiol is made by adding 220 ml of liquid ammonia to a solution of 288 gm cannabidiol-bis-3,5dinitrobenzoate in anhydrous toluene (400 ml) at -70°C in a Parr bomb. The sealed apparatus was mechanically stirred. During five hours the pressure built to 110 psi and the temperature rose to 20°C. The ammonia fumes were released overnight. The product was dissolved in heptane (400 ml) and insoluble 3,5-dinitrobenzamide was removed by filtration. The precipate was washed twice with 150 ml heptane. The heptane solutions were combined and washed with boiling water (5 x 200 ml) and the solvent removed in vacuum to yield 120 gm of a dark oil. Chromatography on 180 gm of this product on 3400 gm of Florisil and elution with 30% chloroform in hexane yielded oily cannabidiol (140 gm).
Crystallization from 30—60° petroleum ether yielded 99.2 gm white prisms, and
recrystallization gave 94.8 gm pure cannabidiol.
Conversion of Pure Cannabidiol to Pure THC
The crystalline prisms of cannabidiol are converted to pure THC utilizing a formula of Roger Adams found on page 2211 of volume 63 of the Journal of the American Chemistry Society. The following is a description of a method for producing pure THC.
Isomerizing the cannabidiol with sulfuric acid
One drop of 100% sulfuric acid was added to a mixture of 1.94 gm crystalline cannabidiol in 35 cc cyclohexane. After refluxing for one hour, the alkaline beam test was negative. The solution was
decanted from the sulfuric acid, then was washed twice with aqueous 5% bicarbonate solution and twice with water. It was then evaporated. This residue was distilled under reduced pressure to yield pure THC with a rotation range of 259° to 269°.
Chonkski
Member
Wow, seriously. Thanks for providing these resources! This is something I have been looking for.
This definitely formed a ton of new questions for a buddie of mine
primeform
Active member
A Cannabis plant 9-tetrahydrocannabinol (THC) isolate according to the present invention was prepared as follows. 2 kg of Cannabis flos (i.e. the flowers) was obtained from Cannabis sativa plants and heated to about 100°C, in order to decarboxylate the cannabinoid acids present in the cannabis flos. The decarboxylated cannabis flos (1.8 kg) was subsequently mixed with hexane (ratio 1 g cannabis flos per 10 ml hexane) in order to extract the cannabinoids from the cannabis flos. The extract was separated from the flos and dried in a rotary evaporator to dryness. The solvent extract (about 600 g) comprised about 55% THC by dry weight.
Subsequently, the dried extract was brought into methanol (ratio 1 g dried extract per 2 ml methanol) and cooled to -10°C and subsequently filtered and centrifuged at 5000 RPM (Beckman Coulter, type Avanti J-26xp) for 25 min at 6°C. To the methanolic mixture obtained, active coal purity p. a. was added in a concentration of 10% by weight on dried extract. The mixture was filtrated and centrifuged again. The solvent extract (about 440 g) obtained comprised about 60% THC by weight of dry matter.
In order to remove the methanol from the mixture, the mixture was brought in a rotary evaporator (Rotavapor® Buchi R-210) and dried with the oil bath temperature of 60°C and rotation in position 5 until vacuum is below 25 mbar. The (partly) dried and viscous mixture with not more than 3 wt % of methanol was brought into a wiped film evaporator (UIC, type KDL- 1 ) with an oil bath temperature of 180°C, water bath temperature of 70°C and a rotor speed of 100 RPM for 45 minutes and dried further such that a refined THC extract of about 380 g was obtained.
The refined THC extract was subsequently fractionated in a high purity fraction with a THC purity > 98%> and low purity fraction with a THC purity of < 20% by means of flash chromatography (Buchi, Fraction Collector type C-660 and UV-detector type C-635) using an ethylacetate / hexane mixture (7% v/v ethylacetate in hexane) as eluent and a pre-packed column of normal silica, with an eluent flow of 250 ml/min, sample flow of 50 ml/min, detection wavelength of 275 nm for 30 min. The fractions were (partly) dried in a rotary evaporator (Rotavapor® Buchi R-210) with the oil bath temperature of 60°C and rotation in position 5 until vacuum is below 25 mbar. The high purity fraction of about 195 g was dried to dryness with a wiped film evaporator (UIC, type KDL-1) with an oil bath temperature of 180°C, water bath temperature of 70°C and a rotor speed of 100 RPM for 45 minutes and the THC isolate obtained of about 160 g was packed in glass syringes for further use.
Subsequently, the dried extract was brought into methanol (ratio 1 g dried extract per 2 ml methanol) and cooled to -10°C and subsequently filtered and centrifuged at 5000 RPM (Beckman Coulter, type Avanti J-26xp) for 25 min at 6°C. To the methanolic mixture obtained, active coal purity p. a. was added in a concentration of 10% by weight on dried extract. The mixture was filtrated and centrifuged again. The solvent extract (about 440 g) obtained comprised about 60% THC by weight of dry matter.
In order to remove the methanol from the mixture, the mixture was brought in a rotary evaporator (Rotavapor® Buchi R-210) and dried with the oil bath temperature of 60°C and rotation in position 5 until vacuum is below 25 mbar. The (partly) dried and viscous mixture with not more than 3 wt % of methanol was brought into a wiped film evaporator (UIC, type KDL- 1 ) with an oil bath temperature of 180°C, water bath temperature of 70°C and a rotor speed of 100 RPM for 45 minutes and dried further such that a refined THC extract of about 380 g was obtained.
The refined THC extract was subsequently fractionated in a high purity fraction with a THC purity > 98%> and low purity fraction with a THC purity of < 20% by means of flash chromatography (Buchi, Fraction Collector type C-660 and UV-detector type C-635) using an ethylacetate / hexane mixture (7% v/v ethylacetate in hexane) as eluent and a pre-packed column of normal silica, with an eluent flow of 250 ml/min, sample flow of 50 ml/min, detection wavelength of 275 nm for 30 min. The fractions were (partly) dried in a rotary evaporator (Rotavapor® Buchi R-210) with the oil bath temperature of 60°C and rotation in position 5 until vacuum is below 25 mbar. The high purity fraction of about 195 g was dried to dryness with a wiped film evaporator (UIC, type KDL-1) with an oil bath temperature of 180°C, water bath temperature of 70°C and a rotor speed of 100 RPM for 45 minutes and the THC isolate obtained of about 160 g was packed in glass syringes for further use.
What you really need is filters that you have to grow in your head yourself. Simple chromatography can do a good job if you start with good material - so don't start building an apparatus for working with anhydrous ammonia yet. The paper showing Adams did not make delta-9 THC is in one of my posts from a couple weeks ago, and I commented on the patent earlier as well.
The same yellow color of the BHO it may have come from indicates to me that the carotenoids are in the Clear, this likely can be scientifically tested and proved with LC/MS with a UV/vis detector. They don't distill with cannabinoids.
Chonkski
Member
I appreciate your concern, but I will not be jumping into anything just yet. Although, my first plan of action it to steam distill using Limonene(perhaps?) as a buffer, instead of water. The boiling point is still 100°f less than the cannabinoids I want. But I still have much more to read and study.
I have also been looking at a Buchi model Rotavapor, because it is half off right now. Which would help a lot with winterization
emeraldcityog
Member
Damn, you guys are still going with this!? I've got pretty good reason to believe the microwave device they use is way out of my - and most people's price range. Along with some other pricey equipment. So I've personally put my attention towards something a little more within my reach - pure dry sift heads. Electrostatic separation.
That said, I sure as hell wouldn't mind it if you guys put this much effort into the unsolved mystery of Skunkman Sam's 99% dry sift heads!
That said, I sure as hell wouldn't mind it if you guys put this much effort into the unsolved mystery of Skunkman Sam's 99% dry sift heads!
L
Luther Burbank
It's almost as if there is no technique, and that by talking about a technique and never explaining it people are forever on the hook wondering.
DeMacho Labs
Member
Have you guys seen xtracted's last ig post with the rotovape? Hmm
jim dankness
Active member
I think they call it 'hyperbaric', not hyperbolic.
Daub Marley
Member
I am on the same page as you with dry sift but Sam's method is not viable. Isolating 99% pure heads at a reasonable scale is like 1000x harder than solvent extraction and Sam's method will yield at best 1% while solvent extraction are ≈20%. Sam deludes himself into thinking that when weed is legal that the price drop would be enough to make his special secret method viable. In actuality keeping it a secret keeps us talking about it like its special, but if he released it then nobody would care.
