02-02-02 19:54
No 264485
Various trials of rearrangement of isosafrole epoxide have transpired. Here's what they got. with 89gms of undistilled isosafrole epoxide. distilled at atmospheric pressure yeiled 15gms of pure Mdp2p and a flask full of polymerized crud. when 89 grams of the same crude epoxide is vac distilled there is yeilded 70 gms of isosafrole epoxide apoun further distillation at atmospheric pressure there is yeilded 62gms of MdP2P which was collected visualy with UV light collecting the fraction that glowed yellow. Bisulfite verufication +
Amination pending
VL_
Decimal_
(Chief Bee)
02-02-02 20:05
No 264488
Very good. What whas the method used for the epoxidation, and what was the yield? Distillation temperature and vacuum used?
And don't forget to report back after your amination.
(Daddy)
02-03-02 13:54
No 264749
If your amination (mention which method pls) turns out ok, then
""which was collected visualy with UV light collecting the fraction that glowed yellow""
is something very handy and new in the arsenal of the underground cook. LT/
PS: what colour did the other fractions (before ketone and after) turned up????? And is there a sudden change in colour or a slowly fading into another shade when fractions change in temp?
WISDOMwillWIN
(Stranger)
02-03-02 19:02
No 264847
Thermometer was broken. that is why the UV was used. swim will dream both again when new one arrives to copnfirm results. there is a few drops of forrun that has a light white glow. only a few drops. Similar to the glow of isosafrole. then the yellow can be seen in stillhead as it begins to come over there is a few minutes from the last drop of the white before the yellow makes it into the condensor. vaccume was 30.2" 167 gms of previously distilled isosafrole tested with nano pseudonitrosite. epoxidised with 1.5lbs of oxone in a 5 gallon bucket.
VL_
(Junior Service Representative)
02-03-02 19:42
No 264867
epoxidised with 1.5lbs of oxone in a 5 gallon bucket.
What did you use to stir this concoction, and at what speed (1800?)? Will a decent magnetic stirrer suffice?
PB
(Hive Addict)
02-03-02 20:13
No 264879
for swim, it was 450g isosafrole, 2L MeOH, 2Gal dH2O, 1lb Oxone, yield was about 350g epoxide.
If you prepare your oxone/MeOH/H2O prior to using, you can filter the precipitate, which is potassium sulfate. Oxone level is not affected by this. This will allow unhindered magnetic stirring other than water resistance.
Real men cook naked.
(Stranger)
02-03-02 21:39
No 264912
Hell yeah thanks. Swim used more oxone because it is 85%.
VL_
(Hive Bee)
02-03-02 21:54
No 264916
Noj, how much extraction solvent did you use for the 400+ grams.
VL_
(Hive Addict)
02-03-02 23:59
No 264957
I honestly don't recall the amount of DCM, but it was likely 3x100mL. When there are no solids in the solution, it is easy to extract. Just let it settle awhile in the sep funnel, tap off the epoxide, and extract the water with DCM.
Stirring was done on a Corning 320 with a 3" bar. Every thing else was like Chromic wrote.
Note that weight was the epoxide. I'll do a rearrangement and bisulfite test in a couple days.
What is the smoke temperature of DOT4 brake fluid?
Real men cook naked.
(Hive Photographer)
02-04-02 04:47
No 265023
From the Höring paper: Ber. 1905, 38, page 2297
Isosafrol-epoxide bp: 140-142degC at 9mm
Isosafrol-ketone bp: 283-284DegC at normal pressure
Yield of ketone by Höring: 80% using destilled epoxide. Water clear oil, almost without smell (the epoxide does smell nice).
(Pioneer Researcher)
02-04-02 06:26
No 265042
Isosafrol-epoxide bp: 140-142degC at 9mm (thanks uemura)
MDP2P 140-145 (9 torr) (thanks Osmium)
It seems difficult to isolate the ketone from the epoxide, right ?
Wich is the color of ketone ? Pale yellow or consitent yellow ?
Very interesing research, thanks.
I'm interested in your UV method. What kind of UV did you use ? The bactericide one hurts your eyes...
(Stoni's sexual toy)
02-04-02 07:17
No 265056
If I ever tried to isomerize the epoxide I'd probably first distill it with an oil pump (low boiling point) to purify, and then do the actual isomerisation in a flask (with an air condenser) under vacuum to limit the (reflux) temperature. I have seen this method being used for the thermal claisen rearrangement of phenolic allylethers, and yields were higher due to less thermal stress. It will take some time though, but better to heat for an hour at 200 or so than 280°C for only a few minutes. This might limit side reactions, I'm pretty sure it is worth a try.
I'm not fat just horizontally disproportionate.
(Chief Bee)
02-04-02 07:30
No 265060
But what about catalysts... Why is noone interested in sprinkling lithium salts or other weak lewis acids on their epoxide?
(Stoni's sexual toy)
02-04-02 07:49
No 265067
Another hard to aquire chem, anhydrous conditions, difficult to get (for some) ethyl acetate.
But the yields of course are clearly in favor of using Li salts.
I'm not fat just horizontally disproportionate.
(Chief Bee)
02-04-02 08:05
No 265069
I did not mean for general use for everybody, but we are now investigating a whole new area of chemical transformations, so it must at least be tried ONCE.
(Stoni's sexual toy)
02-04-02 09:00
No 265081
It's ok boss, nobody stops YOU from trying.
I'm not fat just horizontally disproportionate.
(Hive Bee)
02-04-02 09:03
No 265083
<3x 100ml> arent those the ammounts for a 16 gm extraction. Swim cannot see 300 ml of dcm holding that much oil. more like 3x 1000 ml dcm. swim used 3x1000 for 167 ond only isolated 86gms. No solids present after quick filtering through scotch brite pads. Can the Dcm Ammounts really be reduced that far.
(Chief Bee)
02-04-02 10:06
No 265097
*Sigh*
I get a terribly stressful feeling when I see all the unexplored promising routes and compounds just lying there in my piles of paper, and on this site. Often 90% of the work is done already, a procedure must just be tested with an analog, or with different reaction times, temperatures and/or solvents to optimize the yield and assure purity.
The progress here at the Hive is painfully slow sometimes, people have been discussing the peracetic acid oxidation and LiI epoxide rearrangements for five years, and finally Semtexium did the peracetic last year with excellent results, just as expected. The LiI experiment will probably work just as good. But someone must do it! Even if I worked full time in a well-funded lab, only testing novel procedures, I would never have the time to keep up with the new suggestions to do things, and to optimize the results of a particular reaction to all the interesting precursors we want. If someone wants to make methamphetamine from P2P, they won't just use the appropriate procedure for MDMA and just substitute the MDP2P for P2P - and being the perfectionist I am, I feel it must be tried in practice for us to determine the yield for the particular compound, not just that this-and-that reaction usually gives 60-80% yield with nitroalkenes, I demand to know the exact yields for our five most often used nitroalkenes, as well as footnotes for the compounds when necessary. For example, in my Pseudonitrosite FAQ, there is one general procedure, a table of yields and physical properties, and finally a footnote talking about the neccessary special handling of the asarone derivate. Of course everything should be referenced, and the references checked for pointers to other articles that might help to perfect the reaction.
As I'm the librarian collecting all the good work of the people here and suggesting the most promising avenues to pursue in the future, and I spend my own spare time doing all that reference research, I'm not capable of doing all the labwork myself too. If I would personally try all the reaction varations of our new ideas instead of the theoretical research, then there would a big reduction in novel stuff found for everybody to enjoy. And if I would divide my time between the two, there wouldn't be especially much produced out of any department, as each would only get my attention during half my spare time, and even if I concentrate on only the theoretical side, I still have too little time to produce as much as I want.
Just look at my declining performance at my site (Over 100 new additions in October, 75 in November, 30 in december, and now in January only 11, of which five is just PDF/ZIP files, nothing I have written myself and put any work into!!). And I have not made any practical contributions either, other than taking pictures of ammonium nitrate crystals. If it continues like this, people will be bored with my site as not much new is happening, methods becomes obsolete as I haven't updated the documents with the latest breakthroughs, and I no longer have a purpose here...
I want help with practical tests and theoretical research, I have no possibility to verify everything interesing that is found here, neither practically or theoretically, and just abandon good ideas like we do now is terrible intellectual waste...
(Hive Addict)
02-04-02 10:17
No 265100
VL, if you tap off the bottom oil first, that will account for the majority of the epoxide ~80%. The DCM is to get the rest that may be suspended in solution. The final 100mL DCM is quite clear so it may not even be needed.
Real men cook naked.
(Hive Addict)
02-04-02 10:23
No 265105
Rhodium, in the few years that I have known of your site, I have never become bored with it. It has so much information that I could never absorb it all. But I visit daily and find new things each time. So kudos to you and your efforts!
Real men cook naked.
(Distinctive Doe)
02-04-02 12:06
No 265133
"Just look at my declining performance at my site (Over 100 new additions in October, 75 in November, 30 in december, and now in January only 11, of which fiveare just PDF/ZIP files, nothing I have written myself and put any work into!!). And I have not made any practical contributions either, other than taking pictures of ammonium nitrate crystals. If it continue like this, people will be bored with my site as not much new is happening, methods becomes obsolete as I haven't updated the documents with the latest breakthroughs, and I no longer have a purpose here..."
Hmmm
I wonder if Fractal Flowers beautiful breasts had anything to do with the recent slowdown???
Fully Informed Jury! (http://www.fija.org/)
(Hive Bee)
02-04-02 19:29
No 265288
Noj, does 1 Lb of oxone have the capability to epoxidise 450gms of alkene. Very interested to hear of the ketone work up.
Also Chromic try to use phosphoric acid to make the tma crystals i hear the salt is less hygroscopic.
VL_
(Hive Addict)
02-04-02 19:42
No 265296
I've tried it, the epoxide wasn't destroyed in the distillation. I didn't confirm that I made the ketone (although it seems likely I did), I'm looking for cleaner techniques to go from the epoxide to the ketone. I encourage others to try it tho.
(Junior Service Representative)
02-04-02 20:03
No 265310
What's so bad about the sulfuric hydrolysis? Maybe the black crud that's left in the flask after distillation...
PB
(Hive Addict)
02-04-02 20:12
No 265314
ethyl acetate is available by the gallon in most stores that sell fiberglass and other boat fabricating accessories.
If Pacman had influenced us, we'd run around dark rooms eating pills and listen to repetitive music
(Hive Addict)
02-04-02 20:30
No 265317
I was referring to asarone epoxide.
(Hive Addict)
02-04-02 22:25
No 265361
VL, sorry. It was 2Kg oxone. Let me run it again with detailed note taking and will let you know. I have written down 450g, 355x10 (yellow bottles) 2 gal (but recall adding some more) and 2Kg oxone. I'll make a new thread with an appropriate title when finished. This one is supposed to be thermal rearrangement, which I want to try yet.
Real men cook naked.
(Hive Photographer)
02-05-02 16:16
No 265659
Hi Rhodium,
as Uemura has to agree today: never change a running system...
Another paper on the thermal rearrangement from Mannich ( the Mannich ) "Zu Studien über Adrenalinverbindungen" Ber. ??, ?? (have to check if you want) confirms Hörings statement (Mannich may have however just copied the results, you may know the scientific beesines...)
(Hive Bee)
02-06-02 04:12
No 265910
Make sure you vaccume distill the epoxide. Swim promises that a flask full of crud will ensue with crude epoxide in a thermal rearrangement. did that 450gm batch work up right with those ratios.
VL_
(Hive Addict)
02-06-02 12:23
No 266077
VL, was there anything left in the flask after the Atm distillation? And was the ketone more viscous?
there must be an answer for everything, if only you knew how to set forth the questions
(Hive Bee)
02-06-02 17:33
No 266223
Yes only from the atm distillation of the un distilled epoxide the ketone from the crude rearrangement did not aminate. however the ketone that was produced with the previously vac distilled epoxide did aminate in 66% yeild.there was very little left over in the distillatio it was rubbery and brownish red it dissolved after a while in methanol. the crud from the crude eopxide will still not coome out of the flask.
VL_
(Hive Addict)
02-06-02 18:33
No 266250
Ok, swim has some fluid in the freezer that won't freeze. The H2SO4 hydrolysis was done, then tried a bisulfite adduct, which failed. Tried to aminate anyway, and it failed. So took what was left and distilled at atm pres, leaving a raunchy smelling brown fluid left in flask. I mean it was rank. The distillate looks the same as before though. It is not very visous, like ketones from experience. The blacklight didn't seem to do anything for me. Thermometer was broken, but the hotplate required max heat to get it to come over. I'm not sure what this is anymore with no way to check bp. It smells right, just not viscous. And refractive a bit. I hate to throw it away, since it can't be safrol or iso, and it is unlikely that it is epoxide.
there must be an answer for everything, if only you knew how to set forth the questions
(Pioneer Researcher)
02-07-02 12:03
No 266559
Rhodium , wich catalyst would you use ? LiI and wich else ? ZnCl2, silica gel ?
(Chief Bee)
02-07-02 12:12
No 266564
If I would rank the available alternatives, I'd begin with LiI (or the perchlorate or bromide), followed by MgBr2 (which is said to work satisfactorily, is inexpensive and non-toxic). Next, I would try the Bi(III) salts mentioned in that PDF journal article on my page, just because. My really last choiches would be the stronger lewis acids (FeBr3, AlCl3 etc) as they are probably going to misbehave and tear apart other things of the molecule which we rather would keep if possible (like methylenedioxy rings, methoxy groups, amines etc).
(Stranger)
02-07-02 12:27
No 266571
Rhodium - Still use the ethyl acetate and nitrogen atmosphere and just substitute a molar amount of the salt?
(cheese head)
03-10-02 22:36
No 280494
Does epoxide/diol/glycol freeze in a norml freezer? What is the temp for a thermal rearrangmetn under ATM? Guess a vacuum shouldn't be used for the thermal re arrangment so you can get the exact temp.Thanks
Cheeseboy-a whiteboy with Soul Like a black guy without soul
May The Source Bee With You Always.
(Newbee)
03-11-02 04:28
No 280613
Rhodium,
Can MgBr2 be prepared from Mg(s) and HBr(aq), if so i will give it a whirl, is there any OTC source of Lithium that i can convert to the halogen salt, am not connected to a lab anymore so getting these things involves pulling favours that i would rather save up for the present.
Have some AlCl3 though, any way of weakening it, it has a habit of cleaving ethers so it is worrisome, but i am rather experienced with it so who knows, if it could remain in the solid phase we would be able to control exposure times, i think it would co-ordinate equally well with the methylene ring though, however if mild hydrolysis conditions were used we might convince only the epoxide to rearrange/cleave.
the mag salt seems more promising though, have a think, my inorganic sucks
wacka wacka wacka
(Chief Bee)
03-11-02 10:23
No 280697
Yes, you can make MgBr2 by dissolving magnesium in HBr. Lithium is available OTC in Lithium batteries - a search in the meth form should reveal the details behind opening such batteries and getting the desired Li metal strip.
(Her Majesty, Stoni's Kitty)
03-11-02 13:32
No 280789
Noj, so which is it? 1 pound or 2 kilograms of oxone? (How you can confuse the two is beyond me.) Did you add any buffer? The advice about filtering out the potassium sulfate is great, BTW. However, I'm still perplexed about your results. Are you saying that the yield of ketone was misreported by you earlier in the thread? That the yields of ketone are NOT so good? More information, please.
(cheese head)
03-11-02 16:11
No 280846
Maybe the filtering out of the solids in the OXONE solution has something to do with noj's 'mystery oil' ?
Cheeseboy-a whiteboy with Soul Like a black guy without soul
May The Source Bee With You Always.
(Stranger)
03-11-02 17:08
No 280868
Hope this doesn't sound stupid.. but would it be possible to nuke the distilled epoxide in a microwave to carry out the thermal rearrangement? And watch the reaction with a UV light?
On the 6th day God created man. On the 7th day, man returned the favor.
(Hive Bee)
03-11-02 17:22
No 280877
20 mins on high did nothing to epoxide. Not saying it wont work but need to rig the microwave better before any thing else is attempted.
VL_
(Daddy)
03-11-02 20:24
No 280991
(Rated as: good read)
It's getting confusing in this thread, if I get it right, then noj's tests were not giving amine, V_Lights says he got some amine (or not, not really clear with those ultrashort reportings of him and the others, Flip etc), and I see only one method mentioned, which seem to give a consistent yield, Chromics on Rhodiums pages.
The thermal rearrangement tests (just heat the DISTILLED epoxide at 1 atm to 283-284C, keep it there 20 minutes, then it's ketone, or better, use vacuum at 9 Torr up to 140-145C and reflux with an aircondenser inbetween for approx. 2 hours to get the same ketone, then distill under vacuum to get pure ketone) seems questionable till now, still no real aminations?
Please give me any postnrs if there is one I oversee! I'm getting desperate from the overload of posts lately on the subject of thermal and catalytic (15% H2SO4) rearrangements, and they hop from one thread to another, why not start a new thread with all real factual testreports, and no blahblabla please from people who want attention.
Here's some reading stuff from the Search Engine :
Post 227831 (uemura: "Ketones from Propenylbenzenes via the di-bromides", Novel Discourse) 62 posts, Ketones from Propenylbenzenes via the di-bromides, Uemura's Höring refs etc. Novel forum. After Rhodiums Post 232994 (Rhodium: "Re: Ketones from Propenylbenzenes via the di-bromides", Novel Discourse) it gets again really interesting. ""I don't understand why noone has tested the hypochlorite or hypobromite route to the halohydrin, and then made the epoxide from that with a base. It is OTC, and very simple." I also don't understand, that's layed out in Uemura's starting post up there in this thread.
Post 218193 (Ritter: "LiI catalyzed pinacol rearrangement possible?", Chemistry Discourse) Li catalysed pinacol rearrangement possible? Chemistry forum.
Post 235999 (Chromic: "Asarone epoxidation by Oxone", Chemistry Discourse) Chromic's Asarone epoxidation by Oxone.
Post 241293 (uemura: "Properties of some epoxides", Novel Discourse) Properties of some epoxides, Epoxide Synthesis (described for anethole) and Asarone Epoxide Rearrangement both exellent write ups, wished everybody confirm to this kind of perfectionism and clarity!!!
And Rhodium's Asarone glycol distillation.
TLC techniques by Uemura and Osmium. Plus UV lamp recognision of spots on TLC plates.
Post 241585 (uemura: "Boiling Point Measurement", Chemistry Discourse) Uemura's Boiling Point Measurement, epoxide thermal rearrangment.
Post 265056 (Osmium: "Re: Thermal isosafrole epoxide rearrangement trial", Methods Discourse) Osmium's way of isomerization of an epoxide to the ketone under vacuum.
Post 264485 (Vibrating_Lights: "Thermal isosafrole epoxide rearrangement trials", Methods Discourse) Same thread, Thermal isosafrole epoxide rearrangement trials of Vibrating_Lights (=Flip?):
""Yes only from the atm distillation of the un distilled epoxide the ketone from the crude rearrangement did not aminate. however the ketone that was produced with the previously vac distilled epoxide did aminate in 66% yeild. (V_L)""
Noj however reports a failure to aminate: ""Ok, swim has some fluid in the freezer that won't freeze. The H2SO4 hydrolysis was done, then tried a bisulfite adduct, which failed. Tried to aminate anyway, and it failed.""
V_L tried a microwave: ""20 mins on high did nothing to epoxide. Not saying it wont work but need to rig the microwave better before any thing else is attempted."" Failed till today.
So, conclusion: who got a thermal rearrangement really working, and what yield of amine they got?
Only report is from V_L, 66%. No one else on Isosafrole. A bit meager result to bet your money on.
LT/
PS: And the latest thread Post 243262 (uemura: "Epoxide Rearrangement Example", Methods Discourse) Epoxide Rearrangement Example.
PSII: Post 280823 (cheeseboy: "Re: mdp2p from oxone", Methods Discourse) mdp2p from oxone thread, Cheeseboy claims success, but has not aminated yet, keeps us sitting on the tip of the chair untill he does!
WISDOMwillWIN
(Hive Bee)
03-11-02 22:10
No 281069
First off VL_ is not Flip. Vl used a computer that Flip had been using one day and accidently posted under his name!!!!!
Now
A mix of undistilled isosafrole epoxide/diol from an unbuffered oxone rxn subjected to thermal rearrangement resulted in polymerization and no ketone was produced although the mess of polymerized crap did smell of ketone.
Vac distilled Isosafrole epoxide from a buffered oxone run yeilded ketone. Which in turn yeilded amine.
Apparently in cheese's last unbuffered oxone run it . the 2 hr H2SO4 reflux was only enough to convert the diol to the epoxide. how ever after distilling his epoxide he said he submitted it to thermal rearrangement and yeilded what he believed to be ketone. Lets hope he up dates us on his amination.
VL_
(Daddy)
03-11-02 23:36
No 281093
To clarify I include here again Chromics clear post from the "mdp2p from oxone" thread :
Well, 1-alkene (safrole) to 2-alkene (isosafrole) is obtained by heat and KOH. Then we go onto the oxidation with oxone:
If it's buffered (pH near 7): the 2-alkene becomes the epoxide
If it's unbuffered (pH acidic): the 2-alkene becomes the glycol
(The buffer when used is sodiumcarbonate or -bicarbonate, 85% oxone + 15% -carbonate.)
Then when that's extracted (better stripped of solvents by distillation) and put into the H2SO4 mixture, if it's the epoxide, then it's hydrolysized to the glycol (addition of water, which opens that little epoxide ring). Then the glycol is dehydrated and rearranged by H2SO4 to the ketone by H2SO4. 2hrs of reflux (with stirring) seems to be enough time, yields have always been pretty good.
Then I include your above post, again for clarity reasons, people could get mixed up:
A mix of undistilled (starting from isosafrole) epoxide/diol(=glycol) from an unbuffered oxone rxn subjected to thermal rearrangement resulted in polymerization and no ketone was produced although the mess of polymerized crap did smell of ketone.
Vac distilled (Isosafrole) epoxide from a buffered oxone run yeilded ketone. Which in turn yeilded amine.
Apparently in cheese's last unbuffered oxone run it (. the 2 hr H2SO4 reflux???) was only enough to convert the diol=glycol to the epoxide. how ever after distilling his epoxide he said he submitted it to thermal rearrangement and yeilded what he believed to be ketone. Lets hope he up dates us on his amination.
To clarify more, there seems to be a consensus between various testers at the moment, that there are 3 fractions observed when distilling crude oxonization product: a small forerun of glycol, a big run of ketone, and then a small afterrun of epoxide. Or the other way round.
Now here I can't follow you anymore, how do you know the experienced details of this :
""Apparently in cheese's last unbuffered oxone run it (. the 2 hr H2SO4 reflux???) was only enough to convert the diol=glycol to the epoxide.""
Are you a clairvoyant like Mrs Cleo? Or do you also use HIS computer? 
Don't take that too serious, you have earned it by multiple promisses of schocking writeups, up till now we have to seethe first one yet.
However, I appreciate your posts and work, don't get upset now suddenly, laddie, you'r prolly to busy to write anything more then short posts, go on pls. LT/
WISDOMwillWIN
(cheese head)
03-12-02 12:35
No 281393
VL_ is cheeseboy main man. K Daddy?
Cheeseboy-a whiteboy with Soul Like a black guy without soul
May The Source Bee With You Always.
(Hive Bee)
03-12-02 15:59
No 281531
Vl_ friend swim has been having to deal with stupid personal BS including the loss of most notes and kitchen. Till the dreams can be properly undertaken again a write up would be getto. A getto write up is worth shit. Vl_'s internal trouble sensing unit thus saved him again.
VL_
(Hive Photographer)
03-13-02 02:48
No 281911
Post 280991 (LaBTop: "Isosafrole Epoxide Thermal Rearrangement Review", Methods Discourse)
Thank you Daddy!
(Hive Addict)
03-13-02 05:34
No 281953
I don't recall the amount used now PK. Whatever it was, it was slightly lower than the ratios chromic suggested in his writeup. I believe it was supposed to be something like 2300g oxone but I used 2000g. I may be wrong on that too, since I don't buy the small bottles of pool shock anymore and can't be certain if they were 1lb or 2lb.
The best yield SWIM got from the oxone reaction, was as Chromic suggested in his writeup, and using acid to redissolve the solids in the end. This required an excess of DCM to extract to epoxide.
The suggestion of using no methanol at all was visually accurate, but SWIM has no way to tell what has been made other than visual appearances. It LOOKED like epoxide, but as you stated, it must not have been. I have been frustrated by this reaction ever since I started playing with the amounts.
The main things I think would be helpful would be to mix the water, oxone and methanol together and then filter the precipitate, then proceeding with the isosafrole (buffer if needed).
I apologize if I misled anyone by these posts. I was excited at the time. Who wouldn't be with an OTC synth that was working! I'll leave the reporting to those more apt to do so. And from now on, I will keep notes in accordance with any professional bee. I just hate having incriminating evidence around. Not that I did anything illegal, these were just lucid dreams.
Everyone falls down. It's how fast you get back up that is important.
(Newbee)
03-13-02 21:43
No 282352
>I just hate having incriminating evidence around.
laptop + disk encryption software = secure lab notebook.
try it, you'll sleep better :)
-g
(cheese head)
03-13-02 23:04
No 282389
Cheese's amination via cyano failed. No ketone. Some oil that looks yellowish green that smells like burned fruit, yet not ketone. Ummm wha? Should cheese try again, this time on a small 17gm batch just to have the exact ratios as the write up? Scaling up is dangerous it seems with this one and it seems that buffering is necessary to yield epoxide.unbuffered is a messy situation of tar like cCRUD that you lose your stirbar in FOREVER, until the H2SO4/HCl/acetone combo kicks it's ass.
Faileure, but still lovin' it! now that's sportsmanship!! Thanks for the help everyone, including LabTOP for straigtening things out alot.Cheeseboy-a whiteboy with Soul Like a black guy without soul
May The Source Bee With You Always.
(Hive Bee)
03-14-02 05:59
No 282485
Rhodium,
With the liI salt, is it imperivative to have it completely dr before you use it. I remember in another life we used to dry out PTSA covering it with benzene and then distilling the azeotrope, is ethyl acetate the required solvent to solvate the Li salt or to solvate the epoxide, because if the reaction could be performed in benzene then the hassel of drying the LiI could be overcome by simply distilling for a few minutes and then converting to reflux (no where did I leave that reflix head???)
Any ideas?
Can LiI be made by dissovling Li metal in HI??? (slowly of course)
wacka wacka wacka