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 and......no noticable change!!! Any suggestions as to what is going on?