chemist1243
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diethylamine from household chemicals
Diethylamine from household materials.
Diethylamine can be a difficult-to-procure chemical, because it is a precursor to LSD, making the purchase of diethylamine suspicious unless you have
a very good reason to have it. Thanks to the science madness forum user “madscientist”, there is now a way to obtain diethylamine for lab
purposes. Of course, a good knowledge of chemistry and some equipment will be needed, but other than that the procedure should be fairly simple. all
chemicals needed can be easily purchased at the grocery store. You will need:
1: NaOH (sodium hydroxide, lye.)
2: Distilled water (tap water should work but distilled should be used if available)
3: DEET (this can be found in the form of non-pressurized mosquito spray. Make sure that the concentration of DEET is no less than
95%)
4: 95% ethanol (listen to my directions on this one! this can be found in the form of of ever clear vodka or another type of vodka. As long as it
either says that it is 95% alcohol by volume, or 190 proof, it is 95% pure. Vodka contains almost nothing but water and alcohol. Don’t get
antiseptic alcohol because it contains impurities such as acetone and methanol to deter people from drinking it.)
47ml of distilled water and 50ml of 95% ethanol are mixed together in a 150ml beaker (alternatively, 50ml of water and 50ml of 100% ethanol could be
used, as long as the ratio of water to ethanol is equal, and the volume of the combined solvents adds up to 100ml).
To this solution, 20 grams of pure NaOH is slowly added and dissolved. This is allowed to cool to room temperature.
In the meantime, add 96 ml of DEET to a 250ml 3 necked round bottom flask. Attach a thermometer adapter (with a thermometer in it, obviously) to one
of the side necks on the flask. To the other side neck, add a 150ml addition funnel. Now add 96ml of DEET to the round bottom flask. To the addition
funnel, add the cooled-down alcoholic sodium hydroxide solution. Now On the last neck of the flask, attach a reflux condenser. Start running cool
water through the reflux condenser. Optionally, you can add a stir bar, but I’m sure it will do fine without stirring.
Now let the addition funnel to allow a steady and rapid drip of sodium hydroxide solution. Remember, a steady, but fast, drip. Not a stream. Now
simply allow the addition funnel to drip until all of the sodium hydroxide solution has been added. Once all of the sodium hydroxide solution has been
added, remove the addition funnel, replace it with a stopper, and allow the entire solution to sit for 1:30. By now, you should have noticed an
increase in temperature due to the addition of the sodium hydroxide solution. This evolution of heat is a sign that the reaction is working. If there
was no increase in temperature, then heat the solution in a water bath at 50c for 1:30.
After 1 hour and 30 minutes of either induced heat or just the natural heat from the reaction, you should now be left with a solution of water,
ethanol, a small amount of DEET, and diethylamine. Now
remove the reflux condenser and replace it with a distillation adaptor and a long path distillation column. Turn on the cold-water flow and heat the
solution in a water bath at 56c until the drip of distillate slows significantly or stops completely. 56c is the boiling point of diethylamine, hence
the chosen distillation temperature. I’m not 100% certain on the yields you will get, but it should be easier than trying to buy it.
The collected distillate should be almost 100% pure diethylamine. Distill one more time just to be sure, and then test the PH of the diethylamine
using PH paper. The PH level should be somewhere around 12. Store in an amber glass bottle away from flame, heat, and light. It is a strongly
alkaline, volatile, and flammable liquid.
I cooked this synth up based solely on molar calculations and the thread in which I will link to you below. I got the overall idea of this procedure
based on the thread in the link below, but other than the ingredients used and the water to ethanol ratio, I have come up with myself. Please let me
know how well this synth will probably work, since I haven’t tried it yet. Please do not use this procedure for illegal purposes, as I do not
condone ANY illegal activity.
http://www.sciencemadness.org/talk/viewthread.php?tid=72470
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SWIM
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The water bath is 56 degrees C.
The boiling point of the material to be distilled is 56 degrees C
Why would it even boil if there's no energy going into it at 56 degrees because it has the exact same temperature as the heating bath?
(I saw a pudding recipe like that once. It said to cook something in a double boiler until it boiled. Yeah, good luck with that.)
What about the sodium salt of meta toluic acid.
You've got that just disappearing from the reaction mixture.
What do you mean by a long path distillation column?
What kind of column do you figure on needing to get almost 100% purity distilling from a more or less neutral solution?
[Edited on 8-8-2019 by SWIM]
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Pumukli
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I think the proposed synth would not work. SWIM already pointed out the 56 C thing. In theory it sounds doable but I have the impression that DEET
hydrolysis requires harsher conditions / longer reaction time than your suggested 1:30 hour.
On the other hand you put great effort in balancing the exact ammount of ethanol - why? It is not an analytical chemistry measurement, where you have
to be careful to the Nth decimal digit if possible! It is organic chemistry which is more like cooking food: you don't usually take out a digital
scale to measure salt, just put some in the soup and that's all. Similarly: Between 40 - 60 % ethanol th reaction would have run a similar trajectory.
No need to be exact to 50.000%! 
Similar with NaOH: use a small (few percent) excess compared to the ammount of used DEET and you'll be right. Btw. I heard/read that acid hydrolysis
may be just better for DEET or other amids.
What would be the difference if you mixed NaOH solution and DEET directly instead of the dripping in with a "steady but fast drip"? I think nothing.
Because this DEET hydrolysis seems to be a slow, difficult reaction. I doubt the mixture would considerably heat up by itself!
Heat it to higher than 56 C, prepare to be closer to 70-80 C, especially when approaching the end of the distillation!
What is a long path distillation column? I distilled amines (dimethylamine and pyrollidine) through a 20 cm long water jacketed straight condenser! It
worked. (Dimethylamine was absorbed into cold distilled water.)
I think redistillation of the dried amine (dried with solid NaOH) would be useful.
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