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Hive BB  Methods
Discourse  MeAm::Attempt
one...success??
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| Author | Topic: MeAm::Attempt one...success?? |
| ace NewBee |
 posted 01-24-2000 09:35 PM 
Do I have it or what? I suddenly awoke from a sweaty detox induced nightmare to the following piece of paper. On it was written this cryptic message. In a 250 ml rb, oil bath/stirring hp setup was placed 52 g recrystalized (from water) HTMA(hexamine from camp fuel). 150 ml hardware variety HCL was added w/stirring. Refluxed@104c untill no co2 evolution was noted(2 hrs). Left overnight to cool and a crop of amm chol. was buchnered off. Concentrated under asp. vacuum and cooled, one more crop. Concentrated under vacuum again till yellowish mush was left. Recrystalized w/ hot meoh then washed w/acoh. Left with a yellowish crystals about 45 gms. This mass liquified upon heating. Smells like rotton pussy(or so my gf says! she wont let anyone in the house cuz they will think its her!!lol). Is this the goods(hydrated of course) I have no access to vac. dessicator. how much should I use in my al/hg?? thanks!! |
| takkimitsu Hive Bee |
posted 01-27-2000 12:16 AM
sounds good to me.. the synthesis that is.. not the rotten pussy  . You can get
rid of whatever NH3Cl crystals with an acetone wash. But I dont think
thats necessary until you want to use it.
Just incase I fucked up.. please feel free to correct me anybody ------------------ |
| iudexk Hive Bee |
posted 01-27-2000 02:58 AM
Sounds ok, ummmm, methinks you should just distill for 1st 2 hrs instead of reflux. What I normally do is take all the xtals, dump in MeOH, filter off MeOH, evaporate filtrate and rxtallise filtrate from MeOH to get off-white xtals, then was w/chloroform (removes Me2NH), and finally acetone. |
| Sploofer Hive Bee |
posted 01-27-2000 09:03 PM
any good libary synth encyclepedia outa have the entire data ya are looking for however t would be a wate of my time to type that up......the good stuff would be soluable in alch...and it need be spin dried because vacuming would umm it will auto dessicate maybe it in fact be better to try to salt it up....reading might be a good idea.... I read about the process before however from what I see it seems obvious ya eith er know what ya got or dont the yield seems way down there in the simplified process ya cite..... Each evelution of vacume um something vacumed off some gass perhaps however ya got want to make cl salt it seems hummm maybe if ya simply heat it up disolve the good stuff will be in the alchol it wont percipate to easilly if I rember correctly until it way past the overstaurating point,,, it be a mush as ya described howver some of the mush is not what ya want making distillition seemingly necessary..... |
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