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Pure Oxycodone Synthesis - My Tek

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!!HToBa9dh - Sun, 10 May 2015 19:27:27 EST 4ppVjZXo No.76494
File: 1431300447686.png -(3571B / 3.49KB, 451x323) Thumbnail displayed, click image for full size. Pure Oxycodone Synthesis - My Tek
This was my old one. I'll post it up here in case anyone is interested/ can make corrections on it.
If you want clarification on anything, let me know. The hydrogenation (i think) will be the hardest part for any home chemist, let alone kitchen chemist.

The benefit of this synthesis is that it has no toxic chemicals, doesn't use chromate intermediates, and is made from relatively easy to acquire chemicals.
The downsides are that it requires a lot of chemical knowledge, knowledge on desiccant formations, and is much slower than the sodium dichromate method I have seen used (two refluxes that take up 24hours each are used)
Cod - Codeine
Codo - Codeinone
Oxo - Oxycodone

Workup of Aluminium Isopropoxide
In 250two neck RBF, set one neck up for reflux and one neck up for desiccation. Prepare a drying tube with CaCl2 and link it up to the vacuum adapter in the desiccation neck. Heat all the glassware to an ambient temperature of 80deg C upwards towards the allihn condenser. Proceed to blow air through the drying tube into the flask. Seal off the allihn condenser with a small amount of aluminium foil.
Desiccated aluminium dust (27.98g, 1.00mol) is ground to remove oxide layer and HgCl2 (0.01g) was added. The metal semi-amalgam is added to the bottom of the flask and desiccated isopropanol (250ml, 3.30mol) is injected carefully into the vacuum adapter septum. The vessel is left to reflux for 4 hours.
While still on reflux, the allihn condenser is removed and a 3-way adapter with a thermometer adapter is quickly added. The vacuum is attached to the receiver joint of the 3-way with a one neck 250 RBF while stoppering the side arm of the two neck flask tightly. A distillation is run until only solid aluminium dust remains in the still flask.
A yield of 80% of 1mol aluminium isopropoxide (163.4g) should be achieved.

Oxidation Step
In the same receiver flask of anhydrous aluminium isopropoxide, a desiccated solution of Cod in 100ml of toluene (6g, 20mmol) is added to a solution of aluminium isopropoxide (8.17g, 40mmol) and dried cyclohexanone (9.8g, 100mmol). The receiver flask was set up for reflux and heated for 24 hours.
After cooling the solution to room temperature, 50ml 2.5M hydrochloric acid was added to basify the Codo to Codo HCl and destroy any remaining aluminium. The organic layer was separated and washed with 2 x cc. of water; this layer contained toluene, cyclohexanone, cyclohexanol, and isopropanol. The aqueous layer was combined and 50ml 5M NaOH was added dropwise. The basified solution was washed with 3x 20ml DCM. The DCM was dried under magnesium sulfate and let to evaporate yielding Codo freebase.

9th Hydroxide/ Hydrogenation 1-pot, 2-step Reaction
In a 100ml RBF, 5g of Codo is combined with 10ml 80% formic acid, 5ml 30% hydrogen peroxide, and 1.5ml water. The flask is equipped with a allihn condenser and heated in a water bath at 55° C for 8 hours.
The reaction is taken off heating and cooled in an ice bath to 0° C. 0.5g of palladium chloride is added to the solution and is hydrogenated at 5atm for 24hours. The resulting Oxo solution is basified with 40ml of 30% sodium hydroxide and washed with 2x20ml DCM and 2x10ml diethyl ether. The DCM and ether solutions are dried independently to yield pure Oxo freebase.
107 posts and 5 images omitted. Click View Thread to read.
Ru-lover - Thu, 14 Apr 2016 15:48:37 EST 1yz9Gpwk No.77834 Reply

New isomerization was tried ! With my favorite element Ruthenium black !

***Codeine extraction***

28x60mg of codeine pills with only lactose as excipient are crushed up and dissolved into 20ml dH2O. After a few hours, the suspension is filtered, the filtrate is stirred with 50ml CH2Cl2 and the aqueous phase is made strongly basic with conc NaOH. The aquesous phase immediatly turned to milky white. The two phase system is stirred for 2h. The organic phases is separated and the aqueous one is extracted with 2x50ml CH2Cl2. The org phases are combined, dried over Na2SO4 and rotavapored. After vaccum the oily residue crystallised to for white crystals. Yield 1.25g of codeine freebase from 1.68 g codeine phosphate.


The residue (1.25g codeine freebase) is added into a solution of 2.5 ml H2SO4 2M and 5ml dH2O (H2SO4 0.75 M). The crystals dissolves up on heating to 60-70 °C. 30 mg Ruthenium black is added and the black suspension is refluxed overnight under argon athmosphere. Next day, the ruthenium is filtered on the frit, washed with water and recovered for future use. The slightly yellow filtrate is basified with conc NaOH. The light brown precipitate that immediatly appears is filtered on the frit, washed with dH2O and air dried. The combined filtrate are extracted with 3x50 ml CH2Cl2. After drying and rotavaporing the tan powder are combined and weighed around 1.1g of hydrocodone.

1) Argon athmosphere doesn't seem to be necessairy here, it matters to try without tough.
2) Reaction Time could probably be shorter, TLC is required to determinate the end of the reaction
3) Purity seems to be ok
4) H2SO4 conc. must be as low or lower than 1M to not destroy the substrate after long refluxing time. Its a pity the conc. is not precised in the original patent.
Bombastus !RZEwn1AX62!!xXxJO70U - Thu, 14 Apr 2016 21:23:54 EST V1Ngvki3 No.77838 Reply
Were your filtrates needles or flakes? Also, why were you fixated on ruthenium once more? i have found that palladium works equally and is easier to locate
sorry if you've already answered. uh

Patents never have precise concentrations. They dont' need to. The papers I've found have used codeine HCl with 0.48M sulfuric acid
In my computer projections, because of the catalytic amount needed, I've used down to 0.5M of sulphuric acid with the same yield. it actually got so fucking stupid that I would weigh out a 5ml graduated cylinder, pour sulphuric acid into it, pour it out, then measure the weight of the residual sulfuric acid. then add 5ml of water and calculate the W/V molar mass of the subsequent liquid.
It's silly.

The only issue is that you have to calculate the codeine <-> sulfuric acid acid:base reaction if you're using freebase.

Why are you using deuterated water again?

When it comes to times, my computer projections have never had a TLC monitoring program because it literally happens incredibly quickly. I've gotten the number down to 90 minutes of refluxing and took it off with two separations (one being caffeine, one being co).
Ru-lover - Fri, 15 Apr 2016 18:31:31 EST 1yz9Gpwk No.77843 Reply

In the method its some kind of amorphous crystals or rather more flake-like than needles.

Method with palladium was done a long time ago but did not work out well : dark brown color and several unknown spots. I thought the method was not working well (in fact it was probably too concentrated H2SO4 and long reaction time that destroy the compound in that old method) and I was reading plenty of patent about ruthenium catalyst. You already tried successfully with Pd, so I decided to post the method of ruthenium ;)

In the method dH2O means distilled water, not deuterated.

Ruthenium seems here to be more active than Pd, you need less Ru per g of cod. Did you try other computer projections with a smaller Pd/cod ratio ?

Do you have the solvent infos and TLC rf of cod and HC ?

Do you think the reaction work by skipping the pill extraction, just by dissolving the pills with excipients in H2SO4 and refluxing with Pd or Ru ?

By the way, as you post a method about oppenhauer oxidation of cod I'd like to point out I was reading a patent and I found an interesting oppenhauer oxidation of DHC to cod at ambian temperature with tBuOK/benzophenone in cyclohexane here :

Codeine (11.71 g), benzophenone (48.32 g), 5% palladium on carbon wet (67% water) catalyst (0.37 g), and cyclohexane (57 mL) were charged into a stainless steel autoclave. The autoclave was evacuated and filled with hydrogen. The mixture was mechanically agitated at ambient temperature (25–29° C.) while the hydrogen pressure was maintained at 19–38 psi until the pressure drop caused by the hydrogen consumption stopped. Cyclohexane (120 mL) was charged into the autoclave followed by solid potassium tert-butylate (16.22 g), the mixture was mechanically agitated under nitrogen at ambient temperature for overnight, and then quenched with 1.5N acetic acid (150 mL) with mixing and cooling in the ice bath. The mixture was filtered, aqueous layer was separated and the organic layer was extracted with 1.5N acetic acid (5 mL). Combined aqueous layer was washed with isopropyl acetate (12 mL) and assayed by HPLC. Aqueous solution (176 mL) contains 58.4 mg/mL hydrocodone (90% yield), purity 96 area %.

Coefficient of drag of runners and cyclists

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- Thu, 14 Apr 2016 12:27:35 EST DtZ5lIsF No.77833
File: 1460651255089.gif -(10417B / 10.17KB, 710x531) Thumbnail displayed, click image for full size. Coefficient of drag of runners and cyclists
At what speed (MPH or KPH) does aerodynamic drag become a factor for various items?

I know that for automobiles drag becomes a factor when you're in the 30-40mph ballpark, but what about bicyclists or runners? It's easier to determine the coefficient of drag of, say, an airplane or a car because they're (more or less) static objects, but a cyclist moves their legs and a runner moves their legs and arms.

I'm wondering about this because when I'm on a stationary bike, I'm able to pedal faster with more power when I'm in the typical forward fold versus when I'm pedaling upright-- aerodynamic forces are pretty well negated in this case. The same thing goes for running-- if I'm jogging upright on a treadmill versus leaning forward, I produce more power and speed when I'm leaning forward because my center of gravity has shifted-- but does leaning forward provide any specific aerodynamic benefit for anyone who isn't running as fast as Usain Bolt?
Nell Hagglestat - Sun, 17 Apr 2016 15:28:41 EST 6SGTYI6Z No.77850 Reply
Sounds like a difficult question to answer, but if you're running on a treadmill then do aerodynamics even matter? It seems like they wouldn't compared to normal running.

The Manhatton project is why the Pryamids are really real

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- Sat, 06 Feb 2016 22:12:47 EST NPo+K9eR No.77626
File: 1454814767570.jpg -(119457B / 116.66KB, 736x652) Thumbnail displayed, click image for full size. The Manhatton project is why the Pryamids are really real
If the whole society of America came together to create the A-Bomb and that was an endeavor of a whole society , what evidence of the same thing could be used to disprove that aliens built the Pyramids?
4 posts omitted. Click View Thread to read.
Sidney Fanworth - Fri, 12 Feb 2016 03:54:29 EST X6HIP3d/ No.77651 Reply
Mathematically you can only place one block of a pyramid at a time
Nigger Mucklepune - Sat, 13 Feb 2016 06:21:15 EST +DZfgoAX No.77655 Reply
There's a load of blocks on each layer so you'd be able to work from several different angles bring blocks in. You wouldn't even need to be placing adjacent blocks if you planned it right/on the higher levels. Of course as you go up and it gets narrower this slows down. But most of the blocks will be on the lower levels. You might be placing several remote blocks and joining them up for example. What am I missing?

Hydrogenation without a pressured hydrogenator

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- Sun, 06 Mar 2016 19:24:22 EST 5P3qbCIv No.77713
File: 1457310262241.jpg -(4147030B / 3.95MB, 3000x2590) Thumbnail displayed, click image for full size. Hydrogenation without a pressured hydrogenator
Can this be legit?
Refluxing codeine in an acidic medium with finely grounded Palladium without a hydrogen gas supply to Yield 85-95% of dihydrocodeinone?
Sounds too easy as anyone has an access to a simple refluxing setup, palladium metal, codeine and an acid. Also to my understanding dihydrocodeinone is a fuckload more potent than codeine...
17 posts and 4 images omitted. Click View Thread to read.
Bombastus !RZEwn1AX62!!xXxJO70U - Sun, 20 Mar 2016 14:48:35 EST vbS8CtHn No.77758 Reply
The only way to separate codeine from hydrocodone is either to react all the codeine to hydrocodone.
Or alternatively, you could run a column on them.
press !QUHukXEvkY - Tue, 22 Mar 2016 15:35:02 EST pAeUlupM No.77765 Reply
1458675302660.jpg -(153465B / 149.87KB, 960x960) Thumbnail displayed, click image for full size.
im paaaaaretty sure that crystallization would be sufficient -eventhough they have very similar- solubility as long as theres more product than educt. but then again a short glass tube and some alumina wouldnt cost the world. id have to guess that alumina would be better for the seperation since the codeine is a tad more polar and since sillica tends to fuck with amines. im also guessing it easier to buy and cheaper at a reasonable mesh.

id try and prove my point had i been smart enough to get some Pd/C and if codeine werent sceduled in this shithole.
Ru-lover - Mon, 11 Apr 2016 15:50:28 EST XzFsS2/x No.77823 Reply
Try extraction of the HCodo with bisufite solution. Then crystallise out the HCodo with NaOH.

What have I got here?

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- Sun, 03 Apr 2016 20:58:07 EST SVefPavO No.77797
File: 1459731487924.jpg -(2704061B / 2.58MB, 3264x2448) Thumbnail displayed, click image for full size. What have I got here?
I stumbled upon this bunch of labware from this old dude I've been working for. I'm not sure what all the components are. Aside from basic college chemistry and a couple DMT extractions, I'm pretty much a layman in the chemistry field. But I hope to do something with it, or at least know what its all used for. Any of you science types able to help me identify these?
7 posts and 2 images omitted. Click View Thread to read.
Archie Finningtot - Wed, 06 Apr 2016 07:38:18 EST SVefPavO No.77811 Reply
1459942698064.jpg -(2194792B / 2.09MB, 3264x2448) Thumbnail displayed, click image for full size.
Thanks for the input guys. It looks like i've got a decent setup for clandestine chemistry, its a shame that I probably wont be able to put it to full use. Would some of this be easy/lucrative to sell on CL or something? I have a second separatory funnel and a stand as well that I didn't picture.

I got all this stuff for free, it was just sitting in this guys attic collecting dust and rat shit. If i don't sell it, I'll likely incorporate it into a mixed media art piece, or maybe make molds of some parts and cast copies in ceramic.
press !QUHukXEvkY - Wed, 06 Apr 2016 12:09:50 EST YuS+YrwH No.77812 Reply
isnt lab glassware considered drug paraphenilia or something like that in some parts of the us? i cant recall, maybe im just paranoid

check CL and ebay for an idea of how much you can charge.
i guess you could easily get a hundred bucks, maybe more if you play your cards right and arent in a rush. i have no idea how negiotiating on CL works though
Ian Claydock - Sun, 10 Apr 2016 14:59:36 EST roMD3xgx No.77820 Reply

Chemists are witches out to stir up trouble in the public with their evil craft.

I want to see what the poop sees

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- Wed, 24 Feb 2016 15:48:51 EST ANui6f84 No.77694
File: 1456346931839.jpg -(20795B / 20.31KB, 500x375) Thumbnail displayed, click image for full size. I want to see what the poop sees
How can I turn shit into enegergy I was thinking like a 3 meter dome, shiphon the shit from the sewer before those basteds that fired me from the sewage plant can get there dirty hands all over it, the pretty much lite the gas on fire and covert a diesel generator to take gas, how would one do that?
1 posts omitted. Click View Thread to read.
press !QUHukXEvkY - Fri, 26 Feb 2016 18:36:42 EST ax6SYN1K No.77698 Reply
1456529802353.gif -(2078710B / 1.98MB, 164x275) Thumbnail displayed, click image for full size.
that idea seems very familiar. almost as if its been out into practise for decades.
its a great way to put waste to use

John Gebberwater - Fri, 08 Apr 2016 02:32:24 EST sIdNWEOq No.77817 Reply
That's like one time I splid spot remover on my dog and now he's gone... Lol


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- Sat, 02 Apr 2016 19:43:27 EST CVyPUaOx No.77791
File: 1459640607157.jpg -(18302B / 17.87KB, 525x521) Thumbnail displayed, click image for full size. substitute
ok guys what could I use instead of palladium (II) chloride for catalisys?

this chemical is FUCKING expensive
3 posts and 1 images omitted. Click View Thread to read.
Bombastus !RZEwn1AX62!!xXxJO70U - Tue, 05 Apr 2016 02:21:59 EST Ym/MkWsP No.77805 Reply
nope. palladium black will not do the trick because it requires an oxidation cycle like the regular inert metal coupling reactions.

looks like you're stuck with palladium chloride or find another method.
Ru-lover - Thu, 07 Apr 2016 13:52:58 EST XzFsS2/x No.77813 Reply
try to look on alibaba or other B2B, PdCl2 is 5-10x less expensive there than Sigma or other companies. PdCl2 is a well known product and purity is always good even it comes from china.

Reactions with Tosylates

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- Fri, 25 Mar 2016 04:51:42 EST YfH8FcVI No.77768
File: 1458895902478.png -(12654B / 12.36KB, 200x154) Thumbnail displayed, click image for full size. Reactions with Tosylates
Out of curiosity, would it be possible to react a primary amine with a sulfonyl group (tosylate specifically) and then subsequently use a base followed by a nucleophilic substitution with, say, iodomethane to produce a secondary amine?
1 posts omitted. Click View Thread to read.
Ru-lover - Wed, 30 Mar 2016 19:15:51 EST 1yz9Gpwk No.77778 Reply
Yes you can. The sulfonyl group makes the H more acidic and thus easier to deprotonate. It also locks the nitrogen lone pair avoiding overalkylation.

Help an unmotivated loser out

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- Fri, 01 Apr 2016 15:00:53 EST hqftNCGp No.77783
File: 1459537253692.gif -(11030B / 10.77KB, 197x200) Thumbnail displayed, click image for full size. Help an unmotivated loser out
I realise that this board is mostly used for instructions on how to make drugs in your fucking garage, but since this is also a science board I thought that I would ask you brilliant minds for help.
I have a upcoming project, spanning a year or so, that will entail/connect almost every course I am taking. I am supposed to pick something to create, experiment, etc. and present the result to my professor(s) and peers.
I have seen dudes investigate pharmacuticals, tried to treat salmonella by destroying its flagella with enzymes, etc.
What the hell am I supposed to do?
I might be given access to chemicals, but I do not want to make drugs, even though that would be sweet.
Alice Bicklechot - Fri, 01 Apr 2016 15:32:24 EST NPdGYjgm No.77786 Reply
Is there anything else than sweet sweet drugs that you are even slightly interested in? Preferably something to do with making the world a better place. Great grades coming easily if you do some shit to help african children or make an anti hangover pill.
Start with something not so specific that interests you, do some investigation and then get closer and closer to your ideea until you are drinking champange from a nobel prize while popping anti hangover pills that help african children.

Learning chemistry online

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- Sat, 12 Mar 2016 03:40:46 EST KCS86o4a No.77741
File: 1457772046410.jpg -(15807B / 15.44KB, 559x327) Thumbnail displayed, click image for full size. Learning chemistry online
Hey guys,

I want to get into chemistry. Can you recommend some good, free online courses or something? Or maybe some book(s) that is good for a self-learner? The site study.com offers a free 5 day trial (afterwards the cheapest thing is $50/month which isn't bad), I will give that one a go. On this other site, alison.com are some free courses of introduction to chemistry, which is exactly what I'm looking for, but it looks like these are only videos, I'd rather have something like videos and presentations/written text so I can re-read it and learn it.. you know, just like in college. Yeah I could make my own notices while watching the videos but fuck that noise, I hate making notices. Any suggestions?
Hannah Tootgold - Sat, 12 Mar 2016 17:37:00 EST xxs07y/f No.77742 Reply
Kahn Academy

General and organic chem text books. do the practice problems
Fuck Chondlegold - Mon, 14 Mar 2016 03:11:44 EST hqftNCGp No.77745 Reply
khan academy will have all the chem high school courses
only thing is you wont be able to make cool experiments and shit
schools got access to some sweet fucking chems, dude
Samuel Pibberbutch - Mon, 14 Mar 2016 13:16:59 EST ybs70zkB No.77746 Reply
thanks man, I'll check it out

yeah I know, but I already finished one college and I just started at a new job, I don't have the time right now to start another college. Besides, I don't remember shit from the high school chemistry, so this is a great start for me.

can you id this?

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- Thu, 12 Mar 2015 12:32:49 EST wC5/3Op6 No.76238
File: 1426177969958.jpg -(198139B / 193.50KB, 808x1078) Thumbnail displayed, click image for full size. can you id this?
saw this written down somewhere
curious to what it is
14 posts and 3 images omitted. Click View Thread to read.
Priscilla Huttingtotch - Wed, 09 Mar 2016 08:38:54 EST 5P3qbCIv No.77736 Reply
The picture is from Finland. "Tarjous pizza" means "cheap pizza" roughly translated from finnish to english.
Jenny Binnersetch - Fri, 11 Mar 2016 21:39:50 EST imwkOt2v No.77740 Reply
Maybe it's supposed to be beta-keto-dmt. Like Bk-2cb but with dmt.

Fun chemistry experiments

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- Mon, 29 Feb 2016 18:32:27 EST hqftNCGp No.77699
File: 1456788747344.jpg -(117534B / 114.78KB, 474x325) Thumbnail displayed, click image for full size. Fun chemistry experiments
I remember as a kid I used to mix mr muscle containing NaOH, aluminium and water. A strong exothermic reaction occurs by mixing the NaOH and water. Adding the aluminium instantly reacts with the solution and creates hydrogen gas.
Me and my friends had a blast doing it when we compressed it in a regular old plastic PET bottle (get the pun?)

Are there any similair experiments that causes the same kind of explosive result (made from homemade stuff of course)?

I've heard something about El Dorado soap but idk

I can't really make nitro glycerin like that cool youtube chemist because I don't have access to nitric acid, etc.

And no, officer, I am not a terrorist
2 posts omitted. Click View Thread to read.
press !QUHukXEvkY - Mon, 07 Mar 2016 15:06:33 EST bRQD0jr4 No.77718 Reply
ethanol vapours in a bottle.

just put a small volume of pure ethanol in a big container and shake it around, then wait a bit and light away.

you could use other solvents but it wouldnt look as blue. im also not responsible if you blow yourself up.

Predicting NMR

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- Thu, 03 Mar 2016 04:05:56 EST EP6hRsTc No.77706
File: 1456995956620.jpg -(347960B / 339.80KB, 612x700) Thumbnail displayed, click image for full size. Predicting NMR
What does Anon use to predict NMR?
I'm currently using Mestrenova which is a step-up from ChemDraw but still lackluster.
I'm looking for something that doesn't need to run on a server farm but is still decent enough to serve as a guideline when interpreting spectra.

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