At which point I was stirring with tin foil, and I heard some fizzing. I looked at the tin foil and a white foam was coming off it when out of the liquid. I removed the tin foil immediately and now just shake.

For some reason the flask is extremely hot. 50C exactly. no stirring, no heating, nothing. Its producing heat so I believe hydrolysis is occurring. Because hydrolysis is an exothermic reaction, correct?

That's actually very interesting.  I wonder if AlCl3 is catalyzing the hydrolysis?

Anyone else care to give this a whirl? I have no DEET, nor cash at the moment.

@Agent Madhatter - While erlenmeyer flasks can work as a reflux column on very gentle refluxes, I would recommend setting up a column.  The walls will eventually get hot enough to not condense the material, and Et2NH2 will be the first thing to go once the HCl stabilizes at 20.8% concentration.

"That's actually very interesting.  I wonder if AlCl3 is catalyzing the hydrolysis?"

No! It would be ruining it.  The diethylamine formed by the hydrolysis up to that point would undergo transamidation in the presence of AlCl3 with any unreacted N,N-diethyl-3-methylbenzamide to form Triethylamine and N-ethyl-3-methylbenzamide. It could cause other unwanted by products also like chloro derivatives, generally protic acids are favoured for non-selective 'Hydrolysis'. Unless chemoselective hydrolysis etc is needed then certain Lewis Acids come into play.

Agent Googleless, a round bottom flask is for oil baths etc(sand bath then oil added to fill in the gaps etc). After placing appropriate gauze on your hotplate a flat bottom flask sits straight on the gauze without bathing it.

edit; Those products above are wrong sorry

But the point I was trying to make is that AlCl3 would activate the benzamide toward the wrong sort of attack, ie Lewis acid-base adduct, chloro compound. In hindsight the transamidation will not change the molecules constitution but will definitely have a detrimental effect by holding DEET/Diethylamine in equilibrium and retarding the hydrolysis. The nitrogen on the amide is a good lewis base and chlorodiethylamine could easily be produced instead. The lewis acid base adduct would be a quat cation, which would leave as chlorodiethylamine. Sorry about the wrong products above I knew transamidation played a part but quickly rushed out the wrong products.

The Al problem?
It reacted with the HCl, obviously!

Happens to the best of us, just read anyone of my threads

Interestingly enough plenty of the newer "go-green" or even just the plain newer weed killer sprays contain up to 50% isopropylamine and DEA salts. Some as the salt of glyphosate...well that one is mainly just for the IPA I saw, the DEA salt is probably different...I saw some today and thought I'd share.

Ripped from piglet on DF (we need to get piglet on here...)

step 1 - Add NaOH to diethyl formamide (CAS Number: 617-84-5)
the route goes DEF + NaOH --->HCOONa + NH(CH3CH2)2 + H2O
step 2 - distill off diethyl amine under reduced pressure.

God knows the DEET method sucks, just look on scimad, the rule is the longer the discussion the worst it works practically...
What do you guys think? Not cheap but in the buisness of needing diam, money isn't an issue.

He wont give me the time of day, anyone else want to invite piglet to our community that knows him? He would be accepted with open arms.