To me,getting a orangy toluene extraction from the al/hg it´s equal to things gone 100% right.Obviusly with same amount of freebase to extract,with less volume toluene more orange it will come.If you look at Gonzos´s pictures,the toluene it´s water clear,because it use 700 ml to extract like 20 gr freebase.I use 600 ml to extract near 45 grams freebase,so the toluene it´s way more orange here. If you distill that toluene,you will find a more dirty freebase that you expected,almost dark brown and nothing pretty to deal with.The al/hg it´s a dirty method,and of course,the freebaseobtained it´s dirty too.
I´ve mastered the toluene cleaning after the al/ hg doing that:
1. After extracting the toluene from the sluge,first make ONE WASH WITH LITTLE AMOUNT 10% NAOH solution.You can save a little from the solution you used to basify the sluge on the begining too,Naoh concentration no matters here.It makes the next washes much very easy and clean ,because take off some sluge that it´s still on the toluene.Better too if you have time,will freeze for 30 minutes the toluene to decant some sluge that you can see at room temp.
2. Now you have very clean orangy toluene.wash 3 times with same amount little cold DISTILLED water and finally with brine.The orange stick to the toluene.you will see the toluene only more cloudy because water contained now on it.When you make the last wash,with the brine,let sit more tha usual,no matter layers are well defined,the salt it´s drying the toluene.And now the toluene it will be very clear/transparent orange coloured.The exact order it´s that,if you make again a plain water wash,you will be on the beginig again,with WET toluene.And skip the bicarbonate wash!
3. Dry over MgSo4 .Like now i take things more peacefull
,if i don´t have time,a put toluene and the magnesium on the freeze all night long=the toluene it´s sure dry and no aluminium particules on it.it´s amazing how much sluge it´s on the toluene at room temp that you can see.
4.I never gas now(fucking tricky) ...i extract like much others with 500 ml 5% Hcl solution for 50 gram salt expected on 2 extractions of 250 ml.Here,it´s the only time i shake like mad like 10 minutes for each extraction on the funnel.To me,here don´t work well the stirring method....seems takes more time and yields are low,and on all cases,never got an emulsion here no matter how hard you shake.
5.you get VELVET-RED BLOOD WATER LAYER (more intense on first extraction).
6:and finally:SAVE THE EXTRACTED TOLUENE ,wash again with water 3 TIMES and REUSE FOR THE NEXT EXTRACTION:i´ve used same toluene 5 consecutive times with same great results...if you use on the al/hg again there is no problem with that,you saved a lot money on toluene,and any remaing freebase not extracted will be eXtracted on the next Al/HG.
7.Finally i make a DCM WASH of the acid water solution:it´s take off most of the red colour(what it´s this?
and after evaporation with a fan near the pirex pan,the crystalls are almost transparent without colour,If i don´t make this DCM wash,the resulting crystals are very coloured and not pretty at all.makes a great diference.
8.Quick wash with cold acetone and finish,or recrystallization with acetone flashing if i think the crystals are not pretty enough.
That works for me like a charm!!
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