diethylamine

[flipper]

I found this on this website 

LSD Chemhead

(http://www.angelfire.com/mi3/chemhead/lsdchemhead.html)

Synthesis of diethylamine:

Method #1
From:JP 52036607 19770322 Patent written in Japanese.
Chemicals:

Ethanol (EtOH)
U-Ni-BA catalyst (see MISC section for it's preparation)
aqueous ammonia (NH3)
epsom salt

1-Add 119g of EtOH in a flask.
2-Add 50g of U-Ni-BA catalyst.
3-Add enough aqueous ammonia that contains about 44g of NH3.
4-Setup for reflux, and reflux the solution with a balloon over the flask
and water flow through the condensor as cold as you can get it (to prevent loss of
ammonia vapour) for 6 hours.
5-When reflux time is up, your solution will now have ethylamine, unreacted ethanol, and a little unreacted ammonia as well as water.
6-The solution is filtered of all catalyst.
7-The setup is changed from reflux to distillation, and the ethylamine is distilled out (b.p. 16-17
deg C).
8-The unreacted ethanol is also distilled out and recovered (b.p. 78-79 deg C).
9-The catalyst is regenerated (see MISC section), and placed into a fresh 119g of new EtOH.
10-116g of the above prepared ethylamine is placed into the catalyst/EtOH solution.
11-The flask is setup again for reflux, and the condensor made as cold as possible.
12-Reflux for another 6 hours. Then let cool.
13-Filter out your catalyst, and setup flask for distillation.
14-Distill out any unreacted ethylamine. Then distill out your diethylamine (b.p. 55.5 deg C).
Finally, distill out unreacted ethanol.
15-Oven dry your epsom salt, and add enough epsom to your diethylamine so it adds 1/8th more
volume to your diethylamine.
16-Redistill your diethylamine until it forms a slush with the epsom. The product in the receiving
flask is anhydrous diethylamine.

(The above following synth can probably be done in a microwave setup at a much shorter [like an hour tops] reaction time).

Method #2
from The Hive

Chemicals:

Ethanol (EtOH)
57% Hydrogen iodide (57% HI, see MISC section)
Zn metal
aqueous ammonia (NH3)
epsom

1-Add 119g of ethanol into a flask.
2-Add enough 57% HI to a separate flask so it conatins ~340g of HI.
3-Add a couple pinches of zinc metal to the HI, and reflux it until all of the Zn goes into the solution.
4-Cool the HI back down to room temp, and add it to the ethanol. Reflux solution for 3 hours.
5-When done, setup for distillation, and distill out unreacted ethanol/EtI (ethyl iodide) mixture (b.p. 72-79 deg C).
6-Split the EtI and ethanol fraction in half, and add enough ammonia solution one half the EtI/ethanol mix that contains ~44g of NH3.
7-Reflux that mix with cold ass water in the condensor, and a balloon over the flask to aid in keeping ammonia in, for about 1 hour.
8-When done refluxing, setup for distillation.
9-First distill out the ethylamine produced, then any unreacted EtI/Ethanol.
10-Add the other half of the EtI/ethanol solution to the freshly distilled ethylamine.
11-Reflux this solution for another hour or so.
12-Setup for distillation again, and distill out unreacted ethylamine. Then distill out your diethylamine.
13-Use procedure above to make your diethylamine anhydrous.

(Reflux times in synthesis above can also be shrotened by use of microwaves)

What's wrong with these preparations? Is the yield too low or is it something else?    

[spooky1234]

[cHiLLy]

Flipper, the first one the only thing maybe is the acquisition of the Urishibara catalyst...the second one, no idea. seems like acquisition wouldnt be much of a problem.

[Madog]

damn, did angelfire delete that site or something?

[Rhodium]

biojammer: As the bp of acetaldehyde is 21°C, that wouldn't work. Reductive amination of acetaldehyde (Al/Hg) with aqueous ammonia while cooling to 15-20°C would probably be great, followed by fractional distillation of the extracted amines.

[hypo]

how about this one:

Post 402178 (missing)

(Rhodium: "Alkylamine Synthesis", Newbee Forum)?
not bad, huh?
(FeCl3 is used as etchant by the electronics crowd)

[sYnThOmAtIc]

Why was spookoies post rated as misinforming? I have recieved detailed instructions on the hydrolysis from a respectabel bee that this works. So why was his post rated as misinforming? Is the Off mehtod not actually viable?