LSD chromotography photos

wyndowlicker · Member of the Month

Hey now,

No,the problem is it wont condense fast enough before entering your pump.Its a real bitch.

W.L Razz

IndoleAmine · Dreamreader Deluxe

No way of maybe using less vacuum, and slightly higher bath temp.? Idea

Would increase the effectiveness of your cooling, due to higher temp. diff. - but higher temp isn't good for the substrate, I would guess?

(another idea would be to use an additional condenser on top of the standard rotovap condenser, if this is possible - with buchi rotovaps it is, AFAIK all their condenser joints are 29/32 female at the upper side.. Wink

)

Looks a bit scary though - 1.5 vertical meters of expensive condenser glassware on top of a strange machine... Very Happy

n00dle · Mon Apr 11, 2005 5:18 pm

CDI isnt a standard coupling method like the others is it?
What were the yeilds like?

pybop in DCM gave nothing below 70% analogues in nearly a one pot rxn, can't imagine diethylamine coupling to produce any less. pybRop also is designed for coupling dialkylamines so can produce even better yeilds. tell ya bee that. Smile

*boogies*

methyl_ethyl · Riedel De Haen

DMF is a tricky solvent to condense, I don't have experience with rotovaps as I work with much smaller volumes. However the speedvacs I am familiar utilize roughly the same principle.

Problems people run into when trying to condense DMF:

For some reason many think you have to chill your condensor / vapor trap to near cryogenic levels in order to condense a high boiling point solvent, this is wrong. When I am evaporating DMF under high vacuum, I use a vapor trap set at -5C. For most other applications i.e. lower boiling point solvents / aqueous solutions I use a vapor trap set at -50C. You don't want your DMF to FREEZE! you want it to condense!

Another problem I have seen is the condensation of DMF on lid of the vacuum centrifuge (or for y'all with rotovaps I assume the equivalent would be condensation up stream yet before your condensor). I utilize a centrifuge cover that employs radiant heat to discourage DMF condensation on the lid. I assume rotovap users could insulate your flask or apply mild radiant heat to the flask. Remember just because your substrate/product what have you may be heat sensitive, when you are pulling a good vacuum, applying a little external heat likely will not damage your target, due to evaporative cooling. (Note: this obviously would not apply if your target is light sensitive.)

Well I know there are many more reasons as to why people struggle with high boiling point solvents but that is all I can remember for now. I think the biggest problem is that people are not efficiently condensing DMF but rather freezing it. When it freezes under high vacuum crystals will form at your pump inlet, and crystals formed anywhere else will likely sublime and find there way right into your pump.

At least in my world....

m_e

IndoleAmine · Dreamreader Deluxe

Seems like you're right, the problem isn't a too high bp but rather very high vapor pressure...

Merck index about "N,N-dimethylformamide":

Note the low boiling point at reduced pressure, as well as the sentence "Wherever a solvent with a slow rate of evaporation is required"......
Wink

For freezing n,n-DMF, you would need more than CO2/acetone - dry ice can coll things to -50°C at most IIRC, so you would need liquid nitrogen to crystallize DMF properly in a few seconds...
(since we're on the topic: has anyone ever seen diethyl ether crystals? When you happen to have enough liquid N2, try it! I would LOVE to see a pic of'em.... Laughing

)

BTW with rotovaps, it is hard NOT to achieve radiant heating - the distillation flask rotates in a heating bath, meaning even heat from all sides, as soon as you turn the "rotation speed" knob to make it run...
(and you can also use brown glassware on them! Mine has even a little nipple for attaching an inert gas feed, before venting the whole apparatus and deattaching the flask & residue after distillation is finished... Very Happy

)

i_a

Vibrata_Lumine · Mon Jun 13, 2005 11:37 am

that made me cry man
How you been

timnickbear · Tue Jun 21, 2005 4:10 am

I've been away for a while...working on trying to get info on OB1 in sussex to help a man out if anyone has any info. I have to say fuck yeah to the windowlicker...hope that helps ya hear aphex in your head. What is the approximate amount you have injested mg wise. I am wondering because it seems to be bright in the pix so I would think your guy could get some strong stuffs. I bow to the size of your balls big honcho. was there no oxidation of the product in the beaker?

timnickbear · Thu Jul 07, 2005 6:27 am

Why did the pix go down?

timnickbear · Sun Jul 10, 2005 2:47 am

Does anyone know where the pix went?

wyndowlicker · Member of the Month

Hey now,

I have no idea on what exactly happened to the pictures.Either they were erased or the online harddrive quit posting it for me.Im not sure.Ill get some fresh ones up soon.No you dont get oxidation at any noticable rate as long as you perge your flasks with Nitrogen.

W.L Razz

timnickbear · Sun Jul 17, 2005 4:31 am

Oh my god...I am soooo glad you are still out there!!!! Keep safe WL, as you are our new lord and savior on the subject of LSD. Ok where to start. Some q's from swim. What were the blackish looking specs in your photos in the flask that was shown. Was that mal or tartric acid used with that? What can one do to help the reflux fom turning dark brown? Heat is constant, precursors were purified, and argon is flowing..can't see leaks. It leaves ugly black goo that isn't worth eating...you get spun, but not pleasantly spun. HBWR from methanol extraction thats been forced through a column twice, to get clear liquid(it starts amber), and POCl3 as the coupler in reflux. All done under red photo devoloping light from wolfe. WTF Sad

Have you used argon? A pig to distill the dea was used after the DEET was hydrolized as in the read about dea. It was distilled twice with pig. Swim may quit trying which would suck because he is sooo close. His goo made me trip nuts considering it was the size of a matchhead. Should he get a soxhlet for purification? He says it just turns before his eyes. gtg but l8t wl.

lusitania · Sun Jul 17, 2005 12:00 pm

wow. i am so glad to find someone with incredible knowledge in the rare art of lsd production. This is sorta related, but i thought i'd ask instead of creating a new thread. If i isolate alkaloids from hbwr seeds and get them in a freebase from in solution i should be able to gas this solution and create some salts of lsa right? thx Smile

mk-1 · Sun Jul 17, 2005 6:37 pm

timnickbear, swim does not have first hand experience, but maybe swim can help.
Swim heard of getting "black" acid, and swim have heard of it being in the market. swim believes you need to run it thru a column and rextalize several times from methanol. POCl3 is so old man... move on to pybop, pybrop, CDI or whatever...
There has been something about blackening of product on the hive, cant seem to find it.
Best of luck to you

timnickbear · Wed Jul 20, 2005 3:13 am

Swim has a column and has used it to purify the solution to a clear liquid. The problem occurs during crystallization. He uses the coupler pocl3 as it is available to him...He has tried to use a pig to phase distill the lsa goo into crystals after extraction before the column and has said that a racemerized product occurs, but it will recrystallize and is more manageable than the goo. Methanol and carbon do help clean up his product, however he thinks that the problem is with his rotovap. Over dririte with argon he says he is getting powder to scrape off of a filter disk, however he says it takes a long time to dry.

timnickbear · Wed Aug 10, 2005 2:28 am

still no f'ing pix...this is evil copitulated upon me by the man...You fucking shrubbish bastard and darth asshole.