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| Author | Topic: Quick Wacker Question |
| leno_latrunculus Member |
 posted 10-07-1999 03:42 AM 
Ya, Ya I know you are going to say check the search engine asshole, but I did and I have a couple questions. In the wacker using PdCl2 & benzoquinone, I have noted a few discrepancies(sp?). The post by Spiceboy says 100ml. DMF, 34g. safrole, 11g (is this a typo) benzoquinone and 7g. PdCl2. The Brightstar post says 300ml DMF, 50ml. tap water (why not Dh2o?)120g. benzoquinone, 2g. PdCl2 and 160g.Safrole in 50ml.DMF. Why when BS synth uses only 4.7X the amount of safrole, 3.5X the amount of DMF, .28X the amount of PdCl2 a excess of 10X the amount of Benzoquine is required. I am probably gonna get my ass kicked for even asking this but what gives? I saw so many different molar ratios during my search my head is still swimming. What is the correct amount. I tried this once and it fucked up, I don't want it to fuck up again. Grignards, no problem, but this is a nasty, emulsion intense synth. Please help a stupid idiot like myself. Thanks Leno Latrunculus |
| spitball Administrator |
posted 10-07-1999 03:58 AM
Look asshole, this is a perfectly good question. ( you wanted us to call you asshole, I gathered, right? ok) And you do deserve a good asskicking for asking it. stupid idiot. -spitball-
(I don't have the answer for you, but I'll go kick that fucker, Drone in the ass and get him down here to try and answer your dumbass question. ) heh |
| Osmium Member |
posted 10-07-1999 08:31 AM
I'm not 100% sure, but from what I remember the Spiceboy procedure is way older than the BS synth (no pun  ). Back in the
old days (about two years ago) people used O2 as an oxidiser, could be
that spiceboy used it in his procedure. That could explain why he needed
less. I also think this was one of the first published dreams, so things
might have been non-optimised.
I'd follow the BS synth, it's tested by several bees. |
| Bright
Star Member |
posted 10-07-1999 08:43 AM
You know I love you O. BS |
| pHas3d Member |
posted 10-07-1999 11:25 AM
Yeah... but what is the deal with the "tap" water? Chlorine in the mix help? Or the mineral salts? Or is it the dead (or not so dead) micro organisms?
"tap" is anything but universal.Also, some kids are looking into other fun (evil) replacements for benzo. Would someone be looking for trouble using more angry stuff, or would they be looking at shorter reaction times and less catalyst? O molar equivalent given be a good place to start? stoofid, pHas3d |
| leno_latrunculus Member |
posted 10-07-1999 05:04 PM
Thanks, but what I really need to know is why is there so much benzoquinone, I followed the BrightStar (sorry 'bout the BS, there was no pun intended) Wacker method except I placed everything in a 2000ml. beaker, shitloads of the benzoquinone did'nt dissolve and I had the worst emulsions ever (even after the NaOH washes) is it because of the benzoquinone suckin' the oil up or is it something else. I am one bee who did the Bright Star synth and when I was finished I crystallized everything into a nice white powder which only melted away into a puddle of water (MeNH2 is my suspicion) after 4 hrs. Very discouraging but I am ready to do it again, so maybe Bright Star could have a heart felt one on one on this topic. The synth seems so idiot proof it makes me feel like a peon knowing I am probably the only bee to ever fuck it up. Thanks, Leno Latrunculus |
| The
Alchemist Member |
posted 10-07-1999 11:06 PM
I read this book that stated when the dark rxn mixture is added to the slightly acidic H2O, tons of dark crystals fall out. (Hydroquinone?) A funnel is put on top of my sep funnel and the two layers are decanted as much as possible off the crystals. Now but a peice of filter paper in the funnel which is resting on top of the sep funnel. Throw some DCM in the flask and swirl those dark crystals around and pour in the funnel and let gravity filter. This may take a little while but not that long. Just don't get real thick filter paper. Now wash this stuff on the filter paper a coupl o' times until the DCM that comes through is pretty clear. Here's a trick to distinguish the two layers after the first NaOH wash. The author sez he can never see where the two layers meet 'cuz everything is purple. Give the two layers adequate time to separate. When you take off the bottom layer (DCM/ketone layer), touch the nozzle of the sep funnel to the side of the flask you are emptying into. The DCM layer should be kinda yellowish/clear. Do this SLOWLY. As soon as the slightest hint of watery dark shit is visible, close the valve. Wash the DCM layer 1 to 2 more times and your set. hope this helps |
| Atomicdog Member |
posted 10-19-1999 04:52 PM
Osmium, So are you saying that the spiceboy SRV procedure doesn't work or is a bad one? I've seen the many variations but I'm curious, is the old 50g Saf/ 1g PdCl2/ 40psi regular old air now considered a bust? If it is, what SRV ratios are good if any? |
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