tropine (Stranger)
07-14-03 03:54
No 446941
      Arecoline analogue...freebase success! But....  Bookmark   

So going exactly by the paper, arecoline freebase was successfully synthesized, as a thick yellow oil, which is somewhat soluble in ether.  After diluting the oil in ether, and bubbling HCl gas through, the solution turns white and it appears to have some nice crystals fall out of solution.  However, the majority of the oil stay at the bottom of the flask, with the milky white layer on top.  If this milky white layer is separated and evaporated down (to yield the crystals, as they go right through a filter paper) one is left with a trace of yellow oil in the flask and no crystals.  It seems that these crystals are so small that they go back into the oil phase.  After this anti-climax I re-read the paper and noted that the authors gassed the methanolic solution of the freebase.  So adding about 75% methanol to the ether/freebase solution, the oil immediately went into solution, it dissolves very nicely in methanol.  Then takling this methanol solution, HCl gas is bubbled through noticable change!!!  Any suggestions as to what is going on?
07-14-03 03:58
No 446942
      I meant the chlorophenyl-arecoline product  Bookmark   

was synthed!  But why oh why won't those pretty crystals form!
07-14-03 04:03
No 446943
      I geuss I shoudl also note that I did not  Bookmark   

crystalize before hand from Ethyl Acetate and Hexane like the paper says, maybe this is where the trouble comes from.  It could be that the oil (chlorophenyl-arecoline), being impure has some crap that is unfirendly to cyrstalization...
(Active Asperger Archivist)
07-14-03 16:13
No 447070
      Impurities  Bookmark   

can cause some substances to crystallize more easily, and unfortunately, some become much harder to do the same.  basify, extract, distill, clean the product as the paper states, and then crystallize as they state.  They gave that method for a reason.  Until you've succeeded using their method don't bother with trying other methods.  Experimental can come later after a good sample base has been synthesized for data collection and comparison.

Act quickly or not at all.
07-18-03 05:11
No 448160
      Great  Bookmark   

Once you get past this, be sure to let us know how the bioassay turns out.
(Hive Addict)
07-25-03 01:46
No 449638
      I always thought that gassing freebase cocaine  Bookmark   

I always thought that gassing  freebase cocaine wasn't a widely practiced procedure because the cocaine molecule was very vulnerable to strong acids and bases.  That's why NaOH isn't used to basify the HCl salt.  So just use the crystallization procedure that most people use for regular cocaine freebase.

Post 442507 (andromeda: "Cocaine Base to Hydrochloride Method", Methods Discourse)

It is seductive, way too seductive.             -Eleusis