|
|
| Author |
Message |
java
Consumer
|
| Joined: 07 Feb 2005 |
| Posts: 736 |
| Location: The Mexican Republic |
21796.14 Points
|
|
|
Structure of Cannabidiol..........
Wed Apr 13, 2005 5:38 am |
|
|
Structure of Cannabidiol, XII. Isomerization to Tetrahydrocannabinols'
ROGERA DAMSC, . K. CAIN,W . D. MCPHEEA ND R. B. WEARN
JACS (1941), 2209-2213
pdf |
|
| Back to top |
|
 |
java
Consumer
|
| Joined: 07 Feb 2005 |
| Posts: 736 |
| Location: The Mexican Republic |
21796.14 Points
|
|
|
Old Hive board discussion...........
Wed Apr 13, 2005 5:44 am |
|
|
Back in the old Hive board they had their talk about the subject on this thread......java
----------------------------------------------------------------------------------------------
Author Topic: THC chemistry
drone 342
Member posted 05-05-98 04:57 PM
--------------------------------------------------------------------------------
Hey bees,
Yes, to go out on a tangent, I think its high time (no pun intended) we
get on the subject of thc. With recent advances in THC chemistry, people
can now expect 60-70% yields - twice as much as before! In addition,
friendly scientists around the world have discovered the biological
activity of non-traditional bicyclic rather than tricyclic compounds. Why
hasn't more attention been made to "Adam's 9-carbon compound"?
discussion?
-drone #342
Optimus Prime
Member posted 05-05-98 08:18 PM
--------------------------------------------------------------------------------
Sure I'll discuss it w/ya although I have no friggin idea what ya talkin
about THC = tetra hydro cannibanol(sp?) I suppose???
OP
KrZ
Member posted 05-05-98 09:16 PM
--------------------------------------------------------------------------------
Has anybody tried to isomerize all of your cannabinoids in hash oil into
delta-9 isomer via Sulphuric..
Osmium
Member posted 05-06-98 04:28 AM
--------------------------------------------------------------------------------
Yes, O did it with p-toluenesulfonic acid in pet ether. Isomerization of
dried, blended plant waste and extraction were done at the same time. Cigs
dipped into the pet solution were dried with warm air. Strong material.
drone 342
Member posted 05-06-98 10:41 AM
--------------------------------------------------------------------------------
Has anybody HEARD of adam's 9-carbon compound? By taking regular THC,
lengthening its pentyl chain by to, and adding a couple methyl groups to
the benzylic carbon of that chain (thus producing a 1,1 dimethylheptyl
ligand), you wind up with a cannabinoid allegedly 70 times stronger than
conventional THC.
Optimus Prime
Member posted 05-06-98 11:13 AM
--------------------------------------------------------------------------------
"70 times stronger" ...damnit boy...that would put the heroin dealers out
of buisness. I've never heard of Adam's catalyst but I do believe on the
above note that I should look it up...
OP
weaponx
unregistered posted 05-07-98 06:56 PM
--------------------------------------------------------------------------------
Adam's compound is briefly referred to in Pihkal. This got Shulgin to try
and make Phenethylamine versions of THC. They had no activity, but did
look good on paper. I'd like to know more about Adam's myself. Any more
info Drone? Somewhere to look?
Labrat
Member posted 05-08-98 08:45 AM
--------------------------------------------------------------------------------
Aha, the field of THC chemistry. This is the only field of chemistry which
doesn't interest me at all. I live in Holland and we can buy weed at the
local coffeeshop, so you see there's no need for me to make this difficult
shit from chemicals. If I would, I could make a big batch just from some
seeds.
But for the unlucky ones, there's always the chemical route to get the
THC's.
>Has anybody HEARD of adam's 9-carbon compound? [Not Adam's catalyst OP!!]
Yes siree, I certainly have. In my early days of chemistry, I was
wondering if one could breed weedplants that gave seeds that grew only
females. Ofcourse I checked the chem. literature. That's when I ran into
Adam's dimethylheptylcompound. You seem to have the impression one could
start with regular THC and just add some alkylgroups to it's pentylchain
and voila Adam's cmpd. Certainly this is not true, you'll have to start
with a modified olivetol and condense it with an appropriate group (I
can't remember which, it's so long ago). Anyway, when I was reading an
article about dose-effect relationships of THC analogs, I found that this
Adam's compound is indeed 70 times more potent than THC, but the LD is a
lot lower. Apparently, the Adam compound compared to THC produces a lot
more drowsiness, dry mouth, blurred vision, etc. It's more of a depressant
like quaaludes of barbiturates. But who knows, there are always people
bound to be crazy of this sort of effects (unlike me).
drone 342
Member posted 05-09-98 05:04 PM
--------------------------------------------------------------------------------
Adam's 9-carbon is made just like labrat said, but here's a few more
details. The main problem is, and always has been with the manufacturing
of TCH's, finding a good source for the olivetols or a good method to make
it. The second problem is the yields with traditional methods.
First, the olivetols. This is the way to do it for traditional,
pentyl-chained cannabinoids. hexanal is condensed with acetone to produce
nonenone in an aldol reaction. This is reacted with diethyl or dimethyl
malonate, which forms a cyclic compound. Bromination follows, with a
reflux in HCl. Done.
Second, the newest, bestest way to produce delta-9-THC in 60-65% yields is
a reaction with citral, followed by a dehydration performed in the
presence of a lewis acid catalyst.
The same citral reaction works with the dimethylheptyl compound. Citral
can be made by an aldol reaction involving hexanal and isobutyraldehyde,
followed by a subsequent reaction with acetone (I think, can't remember
this paret off the top of my head so well.) This goes as previously
stated, with the only difference being an reduction of a hydroxy (done
nicely with red p, I assume.)
I'll post refs later. I got the flu, so I'm lazy, but I got an excuse.
-drone 342
RatHead
unregistered posted 05-09-98 05:18 PM
--------------------------------------------------------------------------------
Is that similar to synhexyl?
assholium
Member posted 05-10-98 12:04 PM
--------------------------------------------------------------------------------
Drone, have a good news for you.
Beilstein Netfire. http://www.beilstein.com/netfire/netfire.html
Free. Highly recommended.
Author: Azzena, Ugo; Denurra, Teresa; Fenude, Emma;
Melloni, Giovanni; Rassu, Gloria
Reference: Journal, SYNTBF, Synthesis, EN, 1, 1989, 28-30
Title: A New Synthesis of
1-n-Alkyl-3,5-dimethoxybenzenes (Olivetol
Dimethyl Ether and Homologs)
Abstract: An efficient method is reported for the
synthesis of 1-n-alkyl-3,5-dimethoxybenzenes,
useful intermediates in the synthesis of
cannabinoids, from the readily available and
cheap 3,4,5-trimethoxybenzoic acid.The key
step is the electron-transfer induced highly
regioselective demethoxylation of
1-n-alkyl-3,4,5-trimethoxybenzenes.
CNR: 5642117
delta-9-THC can be obtained by acid-catalysed (p-tolyenesulfoacid)
condensation of verbenol with olivetol. Verbenol easely produced by
oxidation of alpha-pinene with lead tetraacetate (J.Chem.Soc.
p.2235(1961)). Alfa-pinene? Slow fractional distillation of turpentine,
typically it contains near 70-80% of alfa-pinene.
Hope this helps?
Osmium
Member posted 05-11-98 05:10 AM
--------------------------------------------------------------------------------
Olivetol:
Start from 3,5-di-Br-benzaldehyde. React with NaOMe in MeOH/EtOAc with
CuBr catalyst. High-yielding and easy. Proceed with usual Grignard or
whatever to lenghten alkyl chain.
Ref: CA 118; 6734 and T.L. vol 34, 1993, 1007
Piglet
Member posted 06-01-98 08:42 AM
--------------------------------------------------------------------------------
KrZ: I know someone who spent several years during the late 70s' in
Morocco, or more specifically in the Rif mountains. He was part of a group
smuggling hash into the U.K. There method was to extract the THC from the
Kif (rough weed) using IPA and then isomerize it with a few drops of conc.
H2SO4. The mad-strength oil was then made into regular looking hash for
smuggling (In this case by pouring the still-hot liquid hash into the
box-frame of a Land-Rover). Once in the U.K. the hash was cut to produce
commercial shit hash for the dealers. Of course he gor sent down for it in
the end...
D342: I have read several articles about THC analogues with different
length chains. I did think (from memory) that the compound you mentioned
has a VERY long 1/2 life & activity. I don't think I want to be stoned for
2 days! (smoking in the evenings in enough for me). I think that I just
read about the precursors and gave up...
freejon
unregistered posted 07-15-98 01:01 AM
--------------------------------------------------------------------------------
About making it stronger I don't know, but if you stuff enough in a pipe
close one end and blow butane through the pipe out the other end comes the
nicest honsy oil you ever saw time 5 min. wait 30 min with the plate on
your or your girlfriends lap and smoke the way you like best..pure no
other oil no green shit ......
freejon
drone 342
Member posted 07-16-98 04:52 PM
--------------------------------------------------------------------------------
I've always been partial to extracting the oil with alcohol, removing the
chlorophyl and some of the other impurities with activated charcoal,
reaping te goodness that way. I suppose you could go the extra step and
vacuum distill, but usually by that point I'm already pretty content.
Are you talking about gaseous butane extracting the oil, or do you mean
burning, or what? This sounds interesting.
-drone #342
The Cook
Member posted 07-31-98 01:43 PM
--------------------------------------------------------------------------------
YES!! I've been waiting for someone to have a ref on Olivetol! I found a
Chem Abstracts(I think) article on citral (d-limonene-from citrus oil +
Olivetol in cold MeOH with NaOH.
I can't remember what yeilds were... 65% or higher.
PS I use a degreaser at work that's 15% d-limonene. It's $23 for a 5 gal
container!
This means trouble....
PPS Y'all let me know if you need me to post that cold MeOH method.
-later
The Cook
Member posted 07-31-98 01:43 PM
--------------------------------------------------------------------------------
YES!! I've been waiting for someone to have a ref on Olivetol! I found a
Chem Abstracts(I think) article on citral (d-limonene-from citrus oil +
Olivetol in cold MeOH with NaOH.
I can't remember what yeilds were... 65% or higher.
PS I use a degreaser at work that's 15% d-limonene. It's $23 for a 5 gal
container!
This means trouble....
PPS Y'all let me know if you need me to post that cold MeOH method.
-later
Piglet
Member posted 08-02-98 10:17 AM
--------------------------------------------------------------------------------
Citral is a watched item in the UK. I always wondered why...
SleepyMonkey
unregistered posted 08-02-98 01:00 PM
--------------------------------------------------------------------------------
Hey Drone, would you so kindly post your hypothetical oil extraction. It
sounds interesting. I've never heard of going that extra step to remove
the clorophyll by extracting with alcohol along with the use of activated
charcoal. I've always just stopped my dream with the production of the raw
oil but always wondered if it could be cleaned up. Thanks for your time!
drone 342
Member posted 08-02-98 05:32 PM
--------------------------------------------------------------------------------
Damb! I forgot about this thread! I got A LOT of articles on this subject
sitting at home.
Cook, I mentioned this method with citral way back in this thread, but
little came of it. Its an article from Australia, if I remember correctly.
Gimme some time, and I get all my stuff together for y'all on this.
Monkey, the process for removal of chlorophyl is simplicity itself;right
after extracting the "good stuff" from the plant material, filter it, then
add the activated charcoal. Shake it around a little, and it wiull remove
impurities like chlorophyll and other traces of crap.
-drone #342
drone 342
Member posted 08-03-98 10:04 PM
--------------------------------------------------------------------------------
Gentle fellow bees,
I offer you the oportunity to bask briefly in the glory that is the
dronian chem library. Through much struggling and much blood-letting, this
compilation of knowledge has been put together for the greater wellfare of
society. Please enjoy this small fruit of my labor -- a quick review of
the highlights of some of my favorite THC chemistry articles.
Now BASK! Bask, you peasants, BASK!
JACS, 2209-2213 (1941)
cannabidiol->THC (isomerization) kinda useful (cannabidiol is the easiest
precursor to make.)
JACS 217-224 (1971)
isolation of pure THC
JACS 26-29 (1942)
isolation of pure THC
Tet Lett 29, 2511-2512 (1975)
synthesis of olivetol
Chem. Ber. 1845 (1979)
so-so synth of olivetol ethers
Syn Comm 597-598 (1983)
better synthesis of olivetol ethers
JACS 1975 (1941)
really good old-fashioned synthesis report on THC and some analogs; this
is the "dawning" of the Adam's 9-carbon compound
JOC 42, 21, 3456-3457 (1977)
Ass-kicking method for olivetol protuction! This is the way, children!
Really, feel lucky I've given you this, since it was a reall bitch to
elucidate from the literature, and like I said, it just kicks ass.
JACS 28, vol 64 (year?)
iolation purification and acetylation of THC
JOC 16,17 1975
one-step synthesis of THC from chrysanthenol and olivetol
Tet. Let, 26, 8 1083-1086 (1985)
wonderful improvement on THC chemistry describes briefly the use of citral
in the synthesis of THC, as well as a lotof other starting materials.
Aust. J. Chem 1984, 37, 2339-49
This is the bomb! This wonderful paper describes in detail the use of
citral in THC synthesis. This is A MUST for anybody's THC chemistry
library.
JOC 1984, 49, 572-573
More Lewis acid catalyzed THC synthetic fun.
I hope this info helps.
Drone #342,
impaler of infidels,
detroyer of drug policies,
oracle of clandstine alchemy,
resource for all chemistry that is groovy,
humble servent bee of The Hive,
scourge of idiots everywhere,
HAS SPOKEN! |
|
| Back to top |
|
 |
IndoleAmine
Dreamreader Deluxe
|
| Joined: 09 Feb 2005 |
| Posts: 681 |
| Location: Bahamas |
18717.10 Points
|
|
|
Wed Apr 13, 2005 7:23 am |
|
|
Wow, absolutely GREAT!
"By taking regular THC,
lengthening its pentyl chain by to, and adding a couple methyl groups to
the benzylic carbon of that chain (thus producing a 1,1 dimethylheptyl
ligand), you wind up with a cannabinoid allegedly 70 times stronger than
conventional THC."
- I hereby request each and every article that is mentioned in the above Old hiveboard thread, every single bit is welcome... -
Thanks!
(btw bio: the glob turned into something very hard and crisp (at least what is left of it); almost like "colophonium", nice stuff.. )
i_a
Last edited by IndoleAmine on Wed Apr 13, 2005 7:45 am; edited 1 time in total |
|
| Back to top |
|
 |
|
|
|
old hive board text
Wed Apr 13, 2005 7:43 am |
|
|
Your wish is granted,
we are currently making an old Hive Board html document, which will be put into the archive & links section very soon,
It has already been converted, and is just awaiting a few finsihing touches, and it will go up, in all it's glory,
Thankyou to Jackoozi for doing all the html as well,
So i will get to it, and put it up ASAP
syn |
|
| Back to top |
|
 |
THE MOON RULES --1
voted for the moon
|
| Joined: 24 Feb 2005 |
| Posts: 35 |
| Location: Police State |
238.62 Points
|
|
|
hey guys...
Thu Apr 14, 2005 1:37 am |
|
|
Hey indole amine, if your really interested in thc-V come on over to psycotropikal, we have a thread that is untouched and I have tons of questions, like I asked bio , we need a simplified write-up of the procedure for doing so. I just think it would make more since to be writing this tuff over at a site dedicated to this field.
Bio, the problem always found with "hashbuds" is that it is totally hard to work with and market. Its hard to contain. Its hard to convince people that its better then high-quality weed. Its hard to bag up. Its un-economical. I've had freinds try and try to work out a economical formual to work with but it just doesn't happen. The price of the solvents/chems/cannabis doesn't equal into profit of the end result. If youd made it work by all means let me know but for people who have tried a really long time to make it work, it just doesn't all add up. Alotta people use cannabis because they are afraid of chemicals in the first place. So offering somthing like that wouldn't help, they'd want great looking, great smelling, great tasting cannabis, and thats why people want "chronic" and will continue to buy it. I don't see how anyone who regularly smokes high quality cannabis can go back to shwag, I personally would rather go without.
THC-V on the other hand would work ten-fold. If it trully is 500 times more powerfull then THC (thc-V 1/500,000 gm per kilo vs. 1/1,000 gm per kilo) then you would be able to make a solution that you could literally just dose on buds, probally one little drop and it would get you high all day. What would be the yeilds on thc-v, and more importently how much raw material would you have to start with in order to make it? Whats the conversion from regular pure hash oil, to thc-V? I dunno. |
|
| Back to top |
|
 |
IndoleAmine
Dreamreader Deluxe
|
| Joined: 09 Feb 2005 |
| Posts: 681 |
| Location: Bahamas |
18717.10 Points
|
|
|
Thu Apr 14, 2005 3:40 am |
|
|
Isomerizing "hash oil" just converts the inactive cannabidiol (CBD) part into psychoactive delta1(9)-tetrahydrocannabinol (THC), and this makes for much more potency compared to the unisomerized oil. The untreted oil is more sedative, while the isomerized, pure thc oil is more psychedelic.
The delta-V you are talking about is not derived from natural plant extracts, it is a strictly synthetic compound not found in natur, and requires a special synthesis.
You cannot make delta-V from normal THC (sadly ).
(but the isomerized product is still much better than the raw oil, as said - so its still worth the trouble)
i_a |
|
| Back to top |
|
 |
THE MOON RULES --1
voted for the moon
|
| Joined: 24 Feb 2005 |
| Posts: 35 |
| Location: Police State |
238.62 Points
|
|
|
DUH
Thu Apr 14, 2005 4:43 am |
|
|
"By taking regular THC,
lengthening its pentyl chain by to, and adding a couple methyl groups to
the benzylic carbon of that chain (thus producing a 1,1 dimethylheptyl
ligand), you wind up with a cannabinoid allegedly 70 times stronger than
conventional THC."
is where I mistook you thinkin about thc-V
DUH, yea i'm a idiot. so.... the starting material woul be oilvetol (5-(n-amyl)-resorcinol)? I'm totally honest i'm not trying to sound like I know what I'm talking about. Huge reason for the THC chemistry section on psycotropikal is for people (like myslef) to learn from the basics to advances.
I dunno being more of a "cook" then chemist its hard to understand the synthesis. If you could help fellow beginners like myself understand the synthesis it would be great.
Personally I like un iso'd over iso becuase I like the sedation. Everyone likes his or her own though...... |
|
| Back to top |
|
 |
IndoleAmine
Dreamreader Deluxe
|
| Joined: 09 Feb 2005 |
| Posts: 681 |
| Location: Bahamas |
18717.10 Points
|
|
|
Thu Apr 14, 2005 10:22 am |
|
|
"First, the olivetols. This is the way to do it for traditional,
pentyl-chained cannabinoids. hexanal is condensed with acetone to produce
nonenone in an aldol reaction. This is reacted with diethyl or dimethyl
malonate, which forms a cyclic compound. Bromination follows, with a
reflux in HCl. Done.
Second, the newest, bestest way to produce delta-9-THC in 60-65% yields is
a reaction with citral, followed by a dehydration performed in the
presence of a lewis acid catalyst."
Yep - if I would understand it by myself, I would explain to you...
But another thing I just noticed: the isomerization is in fact the formation of a cyclic ether! ( Check the drawings in the article Jave gave us... )
(thats probably why I noticed similarities to diethyl ether production, hehe....)
i_a |
|
| Back to top |
|
 |
jboogie
|
| Joined: 10 Apr 2005 |
| Posts: 2 |
|
580.32 Points
|
|
|
mind if i chime in?
Mon Apr 18, 2005 10:32 am |
|
|
so i was eading this beautiful thread...
so nice to see people taking an interest in the greener things in life.
so this is the latest problem, as you guys have refined the hill-billy recipe into a soup de jor...
if you guys have done this than you no doubt have seent he massive amounts of fat that fuck up my phase..
and being that we are after the oil, which is very similar in properties to the oil, i cant figure out hot to defat the shit..
at first, it wasnt a problem, but the last 2 big ones were half pounds, and it left a fuckin wad of shit on top of the ether phase..
i see the globules trapped, but have no idea how to separate an emulsion like this..
the best i can figure is to let it sit for a week, but that sucks ass...
any suggestions?
i didnt get one [usefull] reply at WD on the sub, thought id drop it here cause its getting bout that time.. |
|
| Back to top |
|
 |
bio
Working Bee
|
| Joined: 13 Feb 2005 |
| Posts: 236 |
|
9718.84 Points
|
|
|
Mon Apr 18, 2005 4:50 pm |
|
|
Hey jboogie! nice to see you around these haunts.
There are many ways to break emulsions and one way usually works better than the others for a particular work-up.
If the crud is floating on top of a lighter than water solvent then you either shook it to hard when washing or if it's diethyl ether, which holds a lot of water (7%?,) some water soluble junk is trapped.
First thing I would do is gently sprinkle powdered salt(NaCl )evenly on the surface. Wait a while at least 15-30 min. This soaks up the trapped water and with a little gentle stirring with a stick it should break. Granular salt tends to fall through too fast but may also work here. If that didn't work then add about 1/3 volume saturated salt water (brine) by squirting and gently swirl the funnel, then invert slowly and vent immediatley.
This should fix it, if not, then you have to do this anyway. Filter through a pleated 25 micron fast paper by dripping slowly enough that the paper doesn't fill more than half way. This filtering alone is sometimes enough and will usually prevent the problem in the first place if you do it when adding the solution to your separating funnel (or any similar device).
............ you no d)oubt have seent he massive amounts of fat that fuck up my phase...........
What you are seeing here is a wax mostly, mixed with a wonderful array of
various pigments, lipids, sugars and god knows what else. To remove most of this and avoid emulsions spray water through the filtered extraction solvent . Don't shake, did I say don't shake? Better to do it over a few times than waiting a week for an emulsion to break.
Also when done cleaning it up if there is some cloudiness then wash thorougly
with brine once or twice. The finished solvent extract should be clear. The cloudiness is residual water which the salt removes.
Good luck and report back. |
|
| Back to top |
|
 |
jboogie
|
| Joined: 10 Apr 2005 |
| Posts: 2 |
|
580.32 Points
|
|
|
can do!
Fri Apr 22, 2005 9:45 pm |
|
|
this next run, boogie is gonna try to locate a clean source of hexane and see if that is an improvement.
is this brake fluid a viable source of hexane for this procedure?
this time he isnt gonna violently stir the mixture..
he will place the carbouy on its side and roll it around to increase phase area, but not mix the two..
and if the shit thats floating on top of my ether is a wax, could it be removed by cold filtration? like just freeze the shit and dump off the hexane? sounds nice in theory, but i dont know if that is right or not..
thanks for all the killer work youve done on this!
fuckin nice!  |
|
| Back to top |
|
 |
IndoleAmine
Dreamreader Deluxe
|
| Joined: 09 Feb 2005 |
| Posts: 681 |
| Location: Bahamas |
18717.10 Points
|
|
|
Fri Apr 22, 2005 11:44 pm |
|
|
Solvent is not that critical I would say; SWIA encountered the same ugly emulsion with diethyl ether as JOE did with hexane, but apparently both seem to clear up very well with powderized NaCl.
When evaporating ether from iso'ed oil, SWIA has seen some precipitate when solvent volume comes down to nothing and the evaporation bowl cools down considerably, but with enough solvent this should not be much of an issue.
If you can see any solids, filter them off! SWIAs butane extracted oil didn't contain solids and dissolved completely in Et2O - so everything that floats is definately crap I would say..
(and waxes should be removed by stirring with activated charcoal methinks)
report back!  |
|
| Back to top |
|
 |
bio
Working Bee
|
| Joined: 13 Feb 2005 |
| Posts: 236 |
|
9718.84 Points
|
|
|
Mon Apr 25, 2005 5:21 pm |
|
|
Hey jboogie; you must be smokin' too much of that good oil you helped me figure out how to make.
Did you try the hair powder hash yet? It is absolutely the best stuff anyone who's tried it says they ever had, nice blond, hard and half weight oil. It took that much to get it to stick together and compacted it in a giant syringe while hot. Next day it was so hard that the syringe barrel (60ml PP) had to be cut off to get the stuff out.
Anyway you said this a couple posts up and I fortunately saved the PM I sent you over at WD in answer to a similar question.
................this next run, boogie is gonna try to locate a clean source of hexane and see if that is an improvement......is this brake fluid a viable source of hexane for this procedure? ..............
So here is an excerpt which may also help some other bees who for whatever reason just don't go out and buy the shit. It is very innocuos and cheap as well.
Hi temp brake fluid is silicone based and the regular stuff I'm not sure but it sure ain't Hexane. If it was you'd have a 30KPSI system that would catch on fire when you hit the brakes. ........
.....Do you prefer working with hexane over ether?...
........Much preferable (Hexanes) to diethyl ether mainly due to the smell, volatility and because it (ether) holds a lot of water (7%??) Petroleum ether is very good although it's maybe too volatile if you want to recycle and don't have a chiller/vapor setup. The 30-60deg pet ether is pentanes / hexanes and is hardly toxic.
Hexane is normal N-Hexane(Bp 69) but the mixed isomers Hexanes(Bp 50-69) are the commercial stuff available in different Bp ranges. It's cheap and non suspicious but you would probably need to get a 50gal drum ($153 a couple years ago).
...............is this a chem shop supplie, or do they sell this at hobby shops?.................
Industrial suppliers like VXXXXXR always have it by the drum maybe even 20L jugs. OTC if you can find it in your area it's the white gas solvent and is damn pure hexane where I live, all boiling below 71deg. But distill it until you find a good brand or just discard everything over say 75deg. Heptane Bp98deg is much harder to get it all out so stay away from that but with a good vac pump it;s really not so bad if properly done.
Pump gas used to be OK except most all has a lot of MTBE these days which can't be separated. If you can still find a high test leaded gasoline without alcohol or MTBE then distill keeping the pentanes and hexanes. I've done it before and the good stuff is maybe 50% Maybe nowdays only race shops have the stuff cause it's not illegal except at the pump. |
|
| Back to top |
|
 |
IndoleAmine
Dreamreader Deluxe
|
| Joined: 09 Feb 2005 |
| Posts: 681 |
| Location: Bahamas |
18717.10 Points
|
|
|
| Back to top |
|
 |
bio
Working Bee
|
| Joined: 13 Feb 2005 |
| Posts: 236 |
|
9718.84 Points
|
|
|
Wed Apr 27, 2005 1:59 pm |
|
|
Yes, it is really good smoke not very harsh at all. I did actually try some! Back in my pothead days long ago it was very rare to find this quality of hash were I was situated at the time.
..........Although his is not yellow but rather black (once again too much oil on too little.. you know Very Happy )..........................
This could also be due to shaking too long, too high temp etc etc. Like I said the half weight oil stuff was a light brown/blond of exceptionally smooth consistency.
Below is a rough draft of how it was done; adapted from an old H thread posted by dPharma if anyone wants to read the entire thing.
......Currently SWIA is thinking about how to get more of that powder...(first tests involved shaking the residual defatted plant matter with more solvent, followed by immediate decantantion of the still turbid liquids, which left a fine yellow dust-like residue upon evaporation. Now how adopt to larger scales?)......
Hmmm seems we're on the same track here! Have a few ideas. Here is one of them. A counterflow classifier (liquid) with layers of screens of different mesh and of course a pump to match the expected flow rate. Buckets poured into the top of a verticle batch unit would work at the University I suppose. Some type of "cotton gin" concept for shredding/grinding and a leaf press or two are needed. Even a simple inclined conveyor with spray nozzles for washing the hairs off might also work.
Haven't tried the defatted residual vegetative matter idea. Sounds like the first thing to try although my sense is that the highest grade "hair powder' is only going to be in the first 2 or 3 fast cold extractions. After that inevitably the undersirable matter starts to predominate. There is a way around this by bleaching/deodorizing as the oil seeds industry
does to the salad oil you eat every day.
This is how it was done by good old Joe.
Cold Hx Extraction Procedure:
1) Fill vessel about 1/2 full with weed that's been well dried (low temp low humidity -dried quickly to < 5% residual water.) Grind but not to a fine powder. (used a blender for shorter than normal) Cover with petroleum ether.
2) Shake vigorously for5 minutes using ambient temp Hx. Immediately decant through a semi fine kitchen strainer to catch coarser pieces.
3) Repeat extraction 2 more times,with fresh cold peth, the third time only shake for 2 min.
4) Pour combined extracts thru a coffee filter then fine filter for workup and solvent recovery.
5) Residue in the coffee filter after air dry is the hair powder.
6) Remove hexane traces with 10mm vacuum thru a short still head after bath rises over 100deg. Continue to 150deg with heavy stirring, flask 1/3 full max. (BTW you will NOT get it all out otherwise)
7) Heat finished clarified oil (shoe polish) and slowly mix with the fine strained hair powder to desired consistency. This took 1/2 weight oil.
So there you have it in rough working form. It's very easy yet cutting corners will reflect directly in the finished product quality.
..................This is an excerpt from the thread here on this site in the H archives, which yields the 'true' fabled' HONEY oil..............................
..............The following method will yeild 'very pure' oil from the 'leaf' material left over after harvesting bud. It will not contain chlorophyll, or other coloring matter.
If done carefully and 'exactly' as presented, will allow the formation of a very convincing (and satisfying) hashish substitute.A 1 liter (quart) mason jar makes an excellent extraction vessel.Larger amounts may be worked if the equipment allows.
1)fill it about 1/2 full with well dried (low temp low humidity -dried quickly) pot leaf, **crushed but not to a fine wder cover the 1/2 liter leaf fragments with petroleum ether.
2)Cover the jar with the lid, close tightly, and shake vigorously for5 minutes.Do not use heated solvent. Do not shake longer.ncap, pour the liquid off, through a kitchen strainer to catchcoarse pieces, and collect in a 2L. jar.
3)repeat extraction 2 more times,with fresh cold peth, the third timeonly shake for 2 min.
The extraction will have a yellowish color with a 'green' cloudytone to it.equip a plastic funnel with a coffee filter, and pour the liquidthrough the filter into another container or the flask to be usedfordistilling solvent. The residue in the filter will be some darkcolor, or even light color, depending on the plant genetics anddevelopment. Save it! it is VERY good stuff.
Te liquid will now be a bright yellow color, with very littlegreenish tint.
Distll the solvent off until only ~50mls. remain. Decant the thickliquid into a pyrex pie plate, rinse the flask with a few ml. pethand add to the pie plateheat the pie plate slightly, while directing the air flow from asmall fan on it's surface. When the last of the solvent is gone,heat a few moments more until a slight smoke indicates an increasein temp. remove from heat and allow to cool.
......Bio does not do this or recomend this overheating in air technique..........
The oil should setup to a very thick paste. It should be darkyellow/brownish and when held up to a bright light will look like HONEY!
Take the residue in the filter paper, seive it several times througha 'fine' kitchen seive, until it's a fine loose powder. (amicroscopic exam at this point reveals millions of tiny hairs).discard any tiny chunks of leaf carried through at the end of seiving.Once the oil extract has solidified, using a narrow putty knife, addabout 2/3 of the powder obtained to the pie plate on top of theextract, and work the powder into the oil. warming the plateslightly will help the two mix together. work it vigorously with theputty knife, until homogenous. It will probably require the entire amt. of powder to make hash ofsuitable consistancy, but may not so add small additional amountsnd work it in. When you like what you've got, form into blocks andstore in a cool dark place until used. Any hair powder left can besaved for another batch. |
|
| Back to top |
|
 |
|
|
|
Powered by phpBB 2.0.11 © 2001, 2002 phpBB Group
Igloo Theme Version 1.0 :: Created By: Andrew Charron
|