================================================================= This file is a part of the 1999 Hyperreal Drug Archives Snapshot. This snapshot is hosted by Erowid and will not be updated after October 1999. The information in these files may be out of date. See Erowid's Psychoactive Vaults for more current info. ================================================================= freya posted 05-28-98 03:22 PM CT (US) ---------------------------------------------------------- Hey there Freya again with a very urgent question. My friends friend tried the CaO method, but had some problems with heating on his lousy hot-plate. Then he wrapped the flasks in alufoil and things seemed to go well, only temperature would not rise to 244C.Because of the foil he could not see inside the flask. Then he tried the advise Strike gave.He filled a small alu-pot with an inch of corn-oil and placed a 250ml flask with the desired 100 ml safrole in it. (safrole was very pure!,it boiled at exactly 232C!)Then he added 15grCaO and 1gr KOH and waited for the oil to reach 244C.But it did not happen, at 242C the oil began to boil and stayed there.Hee let it boil for more then a half hour and then shutted everything off.He thought something was very wrong BUT HE CANNOT FIND THE ANSWER.The CaO used was powdery and very pure, the KOH came in flakes wich he grounded a little. WHAT THE HELL WENT WRONG??????? HELP Thanx in advance for any help........... A frustrated FREYA.................... quirks posted 05-28-98 04:13 PM CT (US) ---------------------------------------------------------- Just a shot in the dark, but maybe your CaO is not dry enough? O. said it's not nessacary to ground the KOH. Osmium posted 05-29-98 03:47 AM CT (US) ---------------------------------------------------------- I said it's not necessary to ground the KOH in my 1%-KOH procedure. Don't know if it is necessary here. 007 posted 05-29-98 09:55 AM CT (US) ---------------------------------------------------------- does the CaO need to be anhydous?? quirks posted 05-29-98 01:37 PM CT (US) ---------------------------------------------------------- I don't know, I just remember someone hypothesizing that it was there as a dehydrating agent. Osmium posted 05-29-98 02:34 PM CT (US) ---------------------------------------------------------- Wet CaO doesn't exist. It's converted into Ca(OH)2, which is useless. So your CaO must be anhydrous. ChemHack posted 06-03-98 12:08 PM CT (US) ---------------------------------------------------------- Osmium: Some hack tried using Ca(OH)2 with KOH dirctly on the kitchen stove just to see what would happen. The temp went to 240C and started smoking like a Bad-Mutha-Fuka. It was an awful smoke that absolutely required a gas mask. The temperature was maintained for 15 minutes during which time a good portion of the liquid was vaporized. The resulting black liquid had a grey mud of Ca(OH)2 on the bottom. From all of this the hack got the bright idea that maybe the KOH is the only important part and the CaO is along for the ride. The hack never tested this hypothesis. quirks posted 06-03-98 02:47 PM CT (US) ---------------------------------------------------------- Is the agricultural lime I see in the hardware store just technical grade CaO or is it Ca(OH2)?? Would lime suffice? Rhodium posted 06-03-98 04:09 PM CT (US) ---------------------------------------------------------- It is only the KOH that is doing the job as isomerizer. One thing that is detrimental to the reaction is water. KOH is 15% water. The CaO reacts with that water, forming Ca(OH)2. Both is needed for a fast, clean reaction. quirks posted 06-03-98 04:14 PM CT (US) ---------------------------------------------------------- Yea yea, but is agricultural lime == slaked lime (Ca(OH)2)?? I don't think it is, which is a good thing cause CaO is very cheap at the hardware store.... ChemHack posted 06-03-98 09:17 PM CT (US) ---------------------------------------------------------- quirks: The Home Drug Manufacture Depot sells lime hydrate in the concrete area. This is Ca(OH)2 so it won't work unless you heat it to around 1000C beforehand to turn it back into CaO. You can tell by looking at it, the hydrate is bright white and the regular CaO is grey. I wonder if Drierite could be used to absorb water instead of CaO ?? Seems like any free water would be released as steam and it isnt soluable in safr or isosafr anyhow....maybe just skip it ?!?! I dunno. Never tried it. quirks posted 06-03-98 10:14 PM CT (US) ---------------------------------------------------------- Yes, but they sell "agricultural lime" too, and I don't know if that's the hydrate or not... Guess there's only one way to find out though. sunlight posted 06-04-98 10:44 AM CT (US) ---------------------------------------------------------- Freya, I think there's nothing wrong. The same happened to me. The reason is there are two isomers of isosafrol, one of them boils at 242 C and the other at 252 C or so. This time you have got most part of this isomer, wich is as good as the other. This happened to me also, but in other dream I got the other isomer. I don't know reasons for this. We said it to you in your previous post. Well, I can be wrong, but smell your oil. It smells more to anise than to safrol. Also a bit of safrol, Yes ? Ok, distill your oil at > 240 C to the end , may be 255 or 248, it's the same. You will get enough pure isosafrol to go on. It's my experience, I did it. Think a bit, if safrol boils at 232, what do you have boiling at 242 C ?. Take a look to a good book or encyclopedia, you can see bp of two isosafrol isomers. Of course, may be I'm wrong, but it seems so clear to me. Next week you will have nitrites procedure detailed. A bit less catalyst, less NaNO2 and less methanol. And easier. ChemHack posted 06-04-98 12:14 PM CT (US) ---------------------------------------------------------- When distilling your post-isomerization product you may want to do this: 1. Distill the safrole off at atmospheric pressure just so that you can be certain that you get it all. Then... 2. Recover the isosafrole under the vacuum so you don't need such high temps. Probably just an old wives tale...do whatever you want.