Topic: lsdotc (Read 244 times)
i remember messing around with this route way back when, found out it's easy just frac distill it and do it SLOW. simple amide hydrolysis...all the DEA i was making from DEET flew out my condenser because i was distilling too fast.i have found by far the easiest and highest yielding method it to partialy hydrolyze the DEET in a solution of ethyl alcohol and potassium hydroxide first. (sealed container as in my synth) then when you go to distill it you must add more KOH (or NaOH) about 25g per 100ml of DEET/EtOH/KOH solution. this will make the diethylamine that distills over fairly anhydrous. there will still be small amounts of water in the form of the azeotrope with the EtOH in solution. fast distillation is fine but you need an air condenser before a graham condenser with at least 5-10°C water running through it. i simply use a homemade air condenser that consists of a 500mm section of 10mm boro glass with a bend at one end for attachment to the boiling flask and the other end blown out and formed to attach to the graham condenser. the whole thing has a 10° slope to keep the diethylamine flowing. once the condenser (graham) has liquid diethylamine in it you must back off the heat to a low reflux otherwise too much pressure will build up in the setup and all your joints could blow apart. this is more prevalent for larger batches using 500ml of deet or more. boiling stones are not absolutely necessary but you have to heat slow to prevent heavy bumping. once you have your first distillate it contains minute amounts of water and a fair amount of EtOH so you have to fractionally distill it. the EtOH has a much higher boiling point than the diethylamine (78°C) so what you should do is start with a clean flask and charge it with 10g NaOH per each 100ml of distillate, add the diatillate and slowly bring up the heat untill you see the vapor start to condense on the thermometer bulb. the temp should be somewhere right around 55°c or slightly less. slowly degree by degree turn up the heat untill you start to see it in the condenser. keep the temp there untill no more comes over. there should be a rise in temperature at that time as there is no more evaporating diethylamine to carry away heat. so stop there and what is in your receiving flask is pure anhydrous diethylamine. store it tightly closed in the fridge to prevent degradation (it will yellow with age but is still good).
