@G.Patton Hey I ran this reaction exactly as written out in this procedure and everything happened as it should up to the point where the post-reaction work up began, and that's where I would like some further clarity if possible.
After 36 hours of stirring at RT following the addition of 100g borohydride, 8L of H20 with 8ml 37% HCL acid were added to the reaction mixture to quench any remaining borohydride with stirring.
Following 10 mins of stirring and 20 mins to settle, (pH was 10) a dark brown freebase formed a bottom layer and was separated from the aqueous layer on top. The aqueous layer remaining in the flask was extracted with 200ml DCM twice, then the combined organic extracts were pooled together.
The aqueous layer was then further basified to pH14 with 30% NaOH solution and allowed to settle. A thin layer of what looked to be freebase oil began to form on top of the water layer, unfortunately after attempting to extract the remaining freebase with another 200ml of DCM, this formed an emulsion that couldnt be broken up and was forced to throw out.
This left roughly 700ml of freebase + DCM (dark brownish red pH is basic for sure). From this point forward, the DCM was rotovapped off and the methanol. (I am thinking this is where the fuck up occurred, should have dried over mgso4 first before evaporating the solvents).
The concentrate was collected and 100g was separated from the main batch of base and dissolved in roughly 4x its volume in chilled IPA (pH was 9) and then gassed with hcl until solution was pH7 but no crystals formed in the solution. The gassed IPA/freebase was put in the freezer along with the main batch of base that remains ungassed.
Where did I go wrong and what can I do to imprve my work up and possibly make my freebase oil a little lighter in colour (any suggestions for washes at certain points in the work up, if so what sort and what order should they be done in). Any idea why crystals did not form when gassed with HCl Gas in the small 100g amount of freebase I trialed this work up with? Any help would be appreciated.