The Vespiary

The Hive => Newbee Forum => Topic started by: k0dog on August 01, 2003, 08:12:00 PM

Title: Thermal rearrangement help!!??
Post by: k0dog on August 01, 2003, 08:12:00 PM

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!!!!!!!!!!!!!!!!!!!!!

Title: My idea...
Post by: k0dog on August 01, 2003, 10:05:00 PM

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

Title: lol!
Post by: hypo on August 02, 2003, 03:20:00 AM

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

do you know the bp of pet ether?  ;D

Title: xylene?
Post by: Rhodium on August 02, 2003, 05:17:00 AM

Of the OTC solvents Xylene might be the best bet, due to its high bp. Not as high as decalin, but still ~140°C...

Title: Boiling points (and other Phys. data) for Xylene
Post by: Aurelius on August 02, 2003, 09:38:00 AM

http://physchem.ox.ac.uk/MSDS/XY/p-xylene.html (http://physchem.ox.ac.uk/MSDS/XY/p-xylene.html)

  (138*C)

http://physchem.ox.ac.uk/MSDS/XY/o-xylene.html (http://physchem.ox.ac.uk/MSDS/XY/o-xylene.html)

  (144*C)

http://physchem.ox.ac.uk/MSDS/XY/m-xylene.html (http://physchem.ox.ac.uk/MSDS/XY/m-xylene.html)

  (138-9*C)

Title: ok...
Post by: k0dog on August 02, 2003, 12:43:00 PM

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?

Title: suggestion
Post by: Rhodium on August 02, 2003, 01:14:00 PM

Extract the formed ketamine with a few portions of 5% HCl, then basify and extract the ketamine freebase into a low-boiling solvent.

Title: alternatively
Post by: k0dog on August 03, 2003, 03:52:00 PM

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..

Title: purification
Post by: Rhodium on August 03, 2003, 05:51:00 PM

You *must* purify it by means of an acid/base extraction + recrystallization of the precipitateed HCl salt...

Title: ok... so
Post by: k0dog on August 03, 2003, 11:05:00 PM

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...