Ok, this is what's going:
1 - This is correct: I used Et2o instead of anhydrous ethanol in 15% ammonia
2 - I DID use maleic acid instead of tartaric acid
3 - I only chromatographed one trial(2nd), which was the most successful one.
I do not think this success is due to chromatography, but due to my LSA. My first LSA hydrolysis did not have satisfying results, I had a few problems w/ the temperature control and with the vacuum pump.
This last addition was made, and no crystals have formed. I guess that my methanol is NOT dry, after all.
Lilienthal, I'm sorry I didnt listen to you. I consider this now a potential cause for the crystals not to come out.
I will dry my MeOH before next procedure. Do you think CaO for a few hours is enough?
Flipper - I am pretty sure you can dissolve the freebase in water and drop it wherever you want, but one should crystallyze it to clean it and to check how much you actually have (how could this be done otherwise?)
Mosh, if you get a successful run, please get to me the details! since I can't, I don;t want to drive you off the way. What I have found is that it seems like everything should be freshly cleaned, dried and distilled, like Buzz's book says. It's really tiring to to all this, but it's not as bad as not having crystals hehehehe
If you want to know how I proceeded for crystallyzation, I only dried the solvents, added a little meoh, (not everything dissolved) then I added a little more (continued dissolving, but some didn't), and then more. Definitely w/ 4ml/gram of freebase will not dissolve the stuff... unless it has to be hot or something...or it takes a hell of a long time. Well, after (almost) everything was in solution ( some stubborn crystals appeared I don't know where from) I added the MeOH (20% maleic acid sol.) and the mixture turned rather quickly into a cloudy mess. Only problem is it continues to be a cloudy mess. I am not sure, but I added some old LSA to complete 3.15 grams, and the solution turned dark in the last 6 hours. The first attempt resulted in a very dark solution also, w/ apparently lower yields. I am guessing that some ET went in there (either ET or other impurities). I still have a few attempts before I cry, I will definitely chromatograph every run from now on.