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| Author | Topic: nutmeg oil raw |
| Bendover unregistered |
posted 06-30-98 05:31 AM
Just soppose that a guy was sitting on 40 gallons of raw nutmeg oil, and as well had 200 grams of Mercury II trifloural acetate and 200 grams of sodium borohydride, and 10 gallons of THF, what would a guy do in his dream? Have all the things but no workable method>????? help will be app. |
| Bright
Star Member |
posted 06-30-98 12:37 PM
Wow...Sounds like a party! Please dispose of the Mercuric Acetate in a proper place (after you use it of course), that stuff is nasty... Step 2 - Buy Total Synthesis by Strike (shameless plug), one of the top ten synths has the route your precursors require. Step 3 - On Rhodiums page, Elusis has a purification procedure for essential oils Well thats a start... Good luck... DON'T TELL YOUR FRIENDS> Bright Star |
| Strike Administrator |
posted 07-01-98 09:37 PM
Thank you, Bright Star. You are very nice. I don't know about this clean-up procedure on Rhodium's site. Is it the one for isolating allylbenzenes? If so one should also take a look at TDK's miracle application of the acetic acid isolation of safrole from safrole-bearing oils. |
| Bright
Star Member |
posted 07-02-98 08:02 AM
I just went there, and its actually a clean up for Sassafrass oil. Oops. The procedure should work however.... I'm afraid that I do not know the percentage of saf in the oil... But after the 1M NaOH wash, a fractional distillation would work.... collect everything that comes over 220->240 range... and keep us informed. Bright Star |
| Bright
Star Member |
posted 07-02-98 08:03 AM
One second thought, fraction distill then do the wash... |
| Cyclops Member |
posted 07-02-98 11:06 AM
On Sassy, Sheep tried 5% NaOH wash, filter, H2O wash, 5x 5% Acetic acid wash (household vinegar!) MeOH then addded H2O. Looks beautiful!! wound up with 79.2% starting weight, sheep hate cooking, always burn shit! Short attention span. |
| quirks Member |
posted 07-02-98 06:20 PM
20-10% mechanical losses pre-distillation is kinda high don't ya think?? I don't bother washing it, there's as much safrole in the wash water as water in the safrole. That's a bad thing. Get relatively pure essential oil to begin with (not essentialoil.com!) If your going to use the safrole, bring the temp slowly up to 234 and hold for five minutes or so. The oil gets a little colour, but it don't hurt things. In fact, if your making isosafrole, and doing the isomerization directly with the sassy then everything will pretty much boil off, then throw all your 100g batches into one container and let settle for a week, and the solids should settle nicely to the bottom leaving a slightly brown clear upper layer that DOESN'T NEED TO BE DISTILLED 4 PERFORMIC!! Also, it seems to take only .5-.7g NaOH / 110g unpurified sassy to get a complete isomerization. IN FACT!! There was like ~3g clumpy CaO/NaOH residue inside one of my flasks that I didn't wash and re-used right away and the safrole started isomerizing even before I put the fresh NaOH/CaO in! Another note, using MeNH3 in Al/Hg from CH2O and NH4Cl, it doesn't really make that much difference if you re-crystalize from ethanol or wash with chloroform, esp the last two concentrations (use the NH4Cl/MeNH.HCl from the 2nd crystalization back in for the next batch, if you use two hotplates you can get a real assembly line going...). Why? Most of the NH3 is going out the top even with a super cold condensor on, and MeNH3 is more electrophilic and soluble anyways. It's OK to do things dirty, spending an extra 24 hours work for what is often LESS, possibly a LOT LESS, yeild and maybe a 5-2% difference in purity, ESPECIALLY if it's non-toxic impurities and if the final product is going to be distilled and acid/based is RETARDED!!! I used to wonder why there was so much stuff on the street that was so obviously unwashed, even in pills (mmmm... stickmen) now I know, cause IT DON'T MATTER!!! But, hey, I'm not saying be irresponsible either. Most of the underground lit. is from chem journals, and in the chem journals they do everything exact and pretty, but for a "production" setup half that stuff isn't nessacary. Spiceboy's got the idea! Comments? |
| jimwig Member |
posted 07-05-98 03:27 PM
i can no longer post thru this oppressive node |
| jimwig Member |
posted 07-05-98 03:29 PM
don't ask what that or this is all about. you need to put about a gallon of sodium borohydride, a pound of ther
HG compound, and a generous quantity of nutmeg oil in containers and
address it to me COD at |
| Cyclops Member |
posted 07-06-98 08:14 AM
Garsh quirks! Sheep had assumed that starting material was between 10-20% non-safole!! Were quite excited with results that weighed what they were theoretically supposed to. Also had bad experiences using oils straight from the bottle, some sheep headed straight over cliff after that experience. Hope this washed stuff works better! |
| quirks Member |
posted 07-06-98 08:40 AM
Maybe sheep could try this: isosafrole from straight-from-the-bottle sassafraass oil, vac filtered, distilled with no forerun - all comes over at the same temp cept for little garbage at the end. Yeild of perfectly clear barely any smell isosafrole: ~85% (of sassy) You could do this with safrole too by just brining it to it's bp then letting cool and then distilling the whole thing. I'm sure there's much more mechanical loss when washing, and it's a hassle. |
| Kaff Member |
posted 08-11-98 02:44 AM
I've read in Total Synthesis and in PiHKAL that nutmeg oil is mostly MYRISTICIN and that is a precursor to MMDA which Strike claims is much more psychedelic than XTC.MMDA synth is in PIHKAL. |
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