k0dog (Hive Bee)
08-01-03 20:12
No 451165
      Thermal rearrangement help!!??  Bookmark   

OK Swim is wondering if anyon could help someone who is dreaming.  Swim is dreaming of thermally rearranging 1-hydroxycyclopentyl-(o-chlorophenyl)-ketone-N-methylimine into ketamine however he has a problem!!! It gives a solvant of decalin...

Now I am wondering why this solvant was choosen to do this rearrangement and if there is another possible answer so that swim may continue to dream in technicolor... Also if any bee knows the ratios for solvant to reactant... much appreciated... on Rhodiums site it says that it's 2.0g in 15ml of decalin however I do believe that is not scaleable at all... Swim would assume less decanlin if I say used 200g I wopuld not uses 1.5 L.. that seesm completely over kill but I could be wrong.. also..

btw I am rewritting a complete freebase--> Hydrochloride rxn write thingy for ketamine because GaRtRoN's is (even tho I helped) not very efficient... anwyays I'll keep the bees posted...

Edit: First off my ketamine conversion thingy is done.. waiting final looking over by another friend tho... also I found that I could also probably use Tetralin, but this does not help me.... grrrr.. also another person said that (decalin and Tetralin
) are used as subsitues for turpintine... but can turpine be uysed as a substitue for them?? help please!!!!!!!!!!!!!!!!!!!!!

"Vanity is defintely my favourite sin"
-Devil's advocate
 
 
 
 
    k0dog
(Hive Bee)
08-01-03 22:05
No 451182
      My idea...  Bookmark   

I am thinking that in this thermal rearrangment it is not that important what solvant I use becasue they do not react at all.  They are merely to tansfer the heat energy to my reactant... and therefore I think that I could probably use any non-polar.. I think I'm gonna try dreaming of petroleum ether, or maybe just Naptha... but before I do this can someone please help me and tell me if I am doing the right thing.. or screwing it up horribly...?? thanks

"Vanity is defintely my favourite sin"
-Devil's advocate
 
 
 
 
    hypo
(Hive Addict)
08-02-03 03:20
No 451216
      lol!  Bookmark   

> I think I'm gonna try dreaming of petroleum ether

do you know the bp of pet ether? laugh
 
 
 
 
    Rhodium
(Chief Bee)
08-02-03 05:17
No 451232
      xylene?  Bookmark   

Of the OTC solvents Xylene might be the best bet, due to its high bp. Not as high as decalin, but still ~140°C...
 
 
 
 
    Aurelius
(Active Asperger Archivist)
08-02-03 09:38
No 451265
      Boiling points (and other Phys. data) for Xylene
(Rated as: good read)
 Bookmark   

http://physchem.ox.ac.uk/MSDS/XY/p-xylene.html  (138*C)
http://physchem.ox.ac.uk/MSDS/XY/o-xylene.html  (144*C)
http://physchem.ox.ac.uk/MSDS/XY/m-xylene.html  (138-9*C)

Act quickly or not at all.
 
 
 
 
    k0dog
(Hive Bee)
08-02-03 12:43
No 451292
      ok...  Bookmark   

I do know the bp of petrol ether is i much lower... actually my new idea is to use kerosine.... becaus ethe bp is according to OTC faq...175-325.. and thta should be ok.... just have to be carful with it tho...

I might actually use ultrasene because it supposedly does not smell... I do have a question tyo.. how would I eliminate the solvant afterwards... Know reduced presure will work... but I have no apparatus that will acheive this.. any other ideas?

"Vanity is defintely my favourite sin"
-Devil's advocate
 
 
 
 
    Rhodium
(Chief Bee)
08-02-03 13:14
No 451298
      suggestion  Bookmark   

Extract the formed ketamine with a few portions of 5% HCl, then basify and extract the ketamine freebase into a low-boiling solvent.
 
 
 
 
    k0dog
(Hive Bee)
08-03-03 15:52
No 451511
      alternatively  Bookmark   

alternatively I could just gas the ketamine fb that was contained within the ultrasene eh?that would make my life just a bit easier.. oh well... anwyas thanks for the help..

"Vanity is defintely my favourite sin"
-Devil's advocate
 
 
 
 
    Rhodium
(Chief Bee)
08-03-03 17:51
No 451522
      purification  Bookmark   

You *must* purify it by means of an acid/base extraction + recrystallization of the precipitateed HCl salt...
 
 
 
 
    k0dog
(Hive Bee)
08-03-03 23:05
No 451560
      ok... so  Bookmark   

ok so.. I take it that ultrasene is an ok choice since it has a high enough boiling point.  I am assuming that this will work... 1 thing left...

ok I have everything needed except what is the thing that hold the oil in? you know the thingy that my round bottom flask is suppose to be like an inch or 2 in...what is taht called I try to find it via UTSE.. but have no clue where to start... sorry for this obvious retared question... but I gotta know...

"Vanity is defintely my favourite sin"
-Devil's advocate