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Discourse  URGENT
Bisulfite/MD-P2P Question...
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| Author | Topic: URGENT Bisulfite/MD-P2P Question... |
| sublime Hive Bee |
posted 01-10-2000 05:32 PM
I dreamt this all last night...it was weird as fuck, but lemme describe it: the benzo-wacker was performed flawlessly, and then all solvent was distilled off, leaving ~200 mL of dark goop which left a VERY neon green residue on flask walls...greener than ever before. It was seeming like my best dream yet. (I prestirred catalyst!) Anyhow, that mix was put in the freezer until a couple days later. It was added to 1000 mL of saturated dH20/bisulfite. I left it to stir and went to bed. By morning, there were TONS of crystals! they definitely looked like chicken fat on close inspection, but looked like green goop when viewing the whole mass of them. I filtered the crystals out of the water. Now I have green/chickenfat goop crystals. How do I clean them up to look only like chicken fat? I assume that there's some hydroquinone in there, or something. Which solvents would be ideal for washing them? I have DCM, IPA, dH20, and Acetone. Once washed, the crystals will be placed into a sep funnel with 10% HCl...this should liberate the ketone, right? I've read conflicting reports about this issue...some say 10% NaOH. Which works here? ----end of dream here--- Thanks all! |
| Sploofer Hive Bee |
posted 01-10-2000 05:49 PM
try using your head the fur will do amazing things to selectivly eliminate oils |
| Osmium PimpBee |
posted 01-11-2000 04:52 AM
I hope you filtered away the black crap as good as possible? I'm not sure but it's possible the bilsulfite might be incompatible with hydroquinone/benzoquinone. Try the washing on a small scale first. I always preferred NaOH to
decompose the bisulfite, because of smell reasons, but that is up to you.
NaOH might be better because you have to wash it with NaOH anyway to
remove the hydroquinone. Divide your chicken fat into several small
portions and try some different workups. Don't forget to post your results
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| APOPLEX Hive Bee |
posted 02-01-2000 12:57 PM
I had a question, Osmium: I worked up a SRV/KRV Wacker ala TS II. I got a red-brown-yellow liquid
after removing the Then I made a soln. of Na2S2O5 in dH2O. I know that this WILL give a aq. soln. of NaSO3 in balance like this: S2O5- + H2O <----> 2 HSO3- So, the sat. aq. soln. should be Ok to meet the ketone I supposed in my above liquid. I dripped some of my liquid into the stirring bisulfite soln. I stirred it about one hour, but NO crystals formed. Only a yellow turbid liquid wich seperates hardly. The SRV-Air-Wacker went exactly like described, so I`m relatively sure that the above oil should contain a lot of ketone. Wrong bisulfite soln. ? What do you think ? Please help ! -------------------
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| Osmium PimpBee |
posted 02-01-2000 01:58 PM
Maybe too diluted? Too much bisulfite solution? I don't know, it should work. |
| Bankrobber Hive Bee |
posted 02-02-2000 01:17 AM
hey sublime, did you wash w/ NaOH(preferably 2-3 times, especially if your new to this ("thing") I,ve personally used bisulfate on filtered, washed(dh2o,NaOH,sodium bicarb, and NaCl), and distilled ketone(when I was in the "beginning", and needed that xtra assurance that I didn't fuck anything up), if you don't do that I suspect that the contaminants can interfere w/ the bisulfate addition(regardless of "promotions" in ts2, by the big guy), I figure from practical exp. that this will not work on contaminated NOT-ketone(I mean by saying this that how often do thigs ever work out when impurities, especially the ones in NOT-ketone prod. are there and the solution is a dirty ass' black, I mean to say it sounds half-ass to me to assume that you aren't going to run into problems, I don't mean that your half-ass SUBLIME, I meant a half-ass bisulfate addition attempt). Anyways one more thought that might be of service dude, your end result of the legal reaction should be way more clear-yellow than a real green(end product should only have hint of green, along with predominate clear yellow). just swish around in see-through container, and no matter wether purified or not you'll see on glass and the solution closest to the glass a slight yellow, that's when you know you've done well( just practical, your original ingredient is clear and know ther's a bunch a' yella, so ya' know your good deed for the day that you promised mom you'd do is now done), take care dude, EVIL ASS' BANKROBBER |
| equarius Hive Bee |
posted 02-02-2000 04:05 AM
BR; So your BISULPHATE addition product reacted just fine? What yeilds? 105%? Did you use NaMetaBiSULPHATE or NaBiSULPATE or NOT some NOT other NOT BiSULPHATE /NOT? Apoplex; Add some EtOH to the solution and it should crash out the crystals.. especially when comming from SRV reactions. And make sure the solution is completly saturated. Disclaimer: Fester (the truth fairy) made me do it. |
| sparks Hive Bee |
posted 02-02-2000 04:24 AM
Sodium bisulfite Synonyms: Hydrogen sulfite sodium; Sodium acid sulfite; Sodium hydrogen
sulfite; Sulfurous acid, monosodium salt; Monosodium sulfite; Sodium
sulfite (NaHSO3) |
| Osmium PimpBee |
posted 02-02-2000 04:48 AM
Solid NaHSO3 does not exist. When evaporating NaHSO3 solutions Na2S2O5 is formed. This is the correct chemical. |
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