Question about distillation is alarmin' me too.
Is it possible to treat w/o it?
Here
https://www.thevespiary.org/rhodium/Rhodium/chemistry/2cb-lah.html
is write-up of purification w/o distilling, as far as I unerstand. Realy it's wrong?
Quote: "Then 20ml 4N NaOH was added slowly. Each portion was allowed to react before the next was added. 60ml water was added and the reaction mixture stirred for an hour or so until it was almost white and granular. The mixture was filtered through a porcelain filter and the filter cake was extracted twice with 50 ml portions of THF in a separate beaker. The organic solvents was combined and evaporated under vacuum. The residue was dissolved in water/HCl (pH=1). The aqueous phase was washed with 3x50 ml CH2Cl2. The organic phase was re-extracted with 50ml HCl/water. Then the combined aqueous phase was made basic with NaOH (pH=14) and extracted with 4x50ml CH2Cl2. The organic phase was dried with K2CO3 and evaporated. The residue (2C-H) was only slightly colored and weighed 16.98g (75%).
A bit more cost effective then earlier methods using LAH I dare say!
According to the original JMC article it is also possible to directly dry the THF solution after filtering off the inorganic lithium/aluminum salts, evaporate the solvent and distill directly to get the freebase. About the same amount of work, and you'll get an even cleaner product."
Pliz calm me. It's very urgent problem to me just now. And I hate vacuum distilling.
Wanna make laugh the GOD? - Tell him about your plans.