After 3 hours of overhead stirring, much black gunk appears splotched throughout the glass.
When I attempted to probe the gunk on the bottom with the stirrer it seemed to be semi-liquid.
Did this reaction fail and thus my toulidine hydrochloride is destroyed?Praxichys - 13-2-2017 at 05:52
First off, I wouldn't rely on an online recipe to cook drugs as a valid synthesis plan.
Which step are you on? It's hard to tell you what you might have done wrong if you haven't even told us what you've done. "Nearly exactly"? Why not
exactly? What did you do differently?
I can only assume you're trying to get around the steam distillation step, which looks tough according to this writeup. IIRC there are better ways of
getting toluidine.
This writeup is abysmal:
Quote:
This procedure must be ventilated out a window or something so the permanganate laden steam doesn't condense on the curtains and make everything pink.
What?Metacelsus - 13-2-2017 at 06:43
That procedure uses iron; I tried that a few years ago and had poor results. Tin worked much better instead.Amos - 13-2-2017 at 07:23
First off, I wouldn't rely on an online recipe to cook drugs as a valid synthesis plan.
Right? And it's almost like we know exactly what they're trying to do!
Very dark coloration is pretty normal after preparing toluidines this way. I'll leave it to you to find a preparation that actually discusses
purification; they're all over the place, at least in more reputable places.dactyl - 13-2-2017 at 13:21
@praxichys
I am on the step just after allowing the iron, nitrotoluene, and water to react and swirl for 2 hours.
There seems to be an implication that the entire procedure on the web link is to be followed. This is not the case. The only applicable steps are
those of the o-toluidine synthesis which is to be used for other reactions.
@Metacelsus I will attempt to procure tin in the future; I considered it a couple of years ago but avoided it for budgetary reasons.
@I am currently think on adding about 500 ml of dilute NaOH aqueous solution to this gunk and perform an in situ steam distillation. Perhaps 100
extra ml of water will be added as the distillation progresses. The author seemed to ignore the hydrochloride possibility dactyl - 13-2-2017 at 13:25
@Praxichys
The main deviation from the procedure was that I used an overhead stirrer which had a single blade (The other blade broke)
If I have misread over the lack or presence of any implication; I apologize.
