Diethyl-Ether = NO Good

[ragga]

Here are 2 different ways of saying the same thing...
the are copied from rhodium's site...
they call for diethyl ether.... fuck.
i could go that route but i don't want to risk a city block on it.
could DCM or petrolium ether work instead? or any other good substitutes?

#1

When the reduction is complete, the catholyte is filtered, evaporated in vacuum and the residue taken up in 300 cc water Unreduced nitrostyrene is extracted sucessively with ethyl acetate and with ether. The crude mescaline hydrochloride solution in a separatory funnel is then treated with a cold concentrated solution of 100 g. of sodium hydroxide and theliberated base exhaustively extracted with ether. The somewhat concentrated
and dried (potassium carbonate) solution is treated with a stream of dry hydrogen chloride and the separated hydrochloride twice recrystallized from absolute alcohol.

#2
After the finished reduction, the contents of the cathode cell was filtered and dried under vacuum. The remainder was then dissolved in 300ccm water. Any remaining unchanged nitrostyrene was removed by twice shaking it out with ethyl acetate. The ester in the solution was then removed by shaking out once with diethyl ether.

The liquid thus obtained of chloride of mescaline was then put in a separating funnel which had ether added. The amine was freed with a cold concentrated solution of technical sodium hydroxide. The solution obtained, after extracting four times with ether, etc... pure hcl salt
 

[ragga]

let me try again.
can i use somethiing else other than diethyl ether in this?

[foxy2]

Just Use the starting fluid, it ain't that bad IF you are careful.  My guess is you are in an apt and paranoid about burning it down. Thats probably smart.

For#1
Use a nonpolar such as tol or DCM to extract the freeebase M should work. Read every M synthesis ya can find, look for the solvent they use to extract the freebase this would be the way to go if you lack any chem experience.  Or trial and error can be done fairly easily.

However i would prolly still use ether to do the initial reaction clean up. This should be relatively easy, just have a fire extinguisher on hand and right when your done take the ether outside and dump it on the street somewhere so it can evaporate.  Don't work near ignition sources such as piolet lights, small electric motors.

One other thing
This question is more appropriate for the newbee forum



Happy New Year

[uemura]

ragga: read other references and you find: M is not very soluable in ether anyway.

[improv_chem]

Just finished reading a book on cacti (the funky kind) and found out that you can make nice mesc-sulfate crystals by disolving the sulfate salt in distilled water then cooling the solution in a fridge.  (The sulfate salt is only a little soluable in cold water)If you use sulfuric acid soltuion on the freebase extracts instead of HCl, that is.  I have never had any trouble with diethyl-ether starting fluid for a solvent, but then i NEVER heat the stuff up or have any flame or sparks near by.
Just use some common sense when playing with ether and don't try and distill it.


It's all just a dream, I hope i don't wake up because of that incessent buzzing sound...

[uemura]

Yes, in certain circumstances the sulfate salts are better to deal with. However: make sure you recrist your sulfat salt! If traces of free sulphuric acid remain, your product gets destroyed over the long time.

What bothers Uemura more than the fire danger of ether are its peroxides! Destilling ether IS NOT A BIG DEAL if you use
a water bath for heating
a fully glas destillation apparatus with an ice-cooled receiver
a tube going out-of-window or at least to the bottom of the floor AND
never destill to dryness

[improv_chem]

Yes, peroxides are exactly why i don't distill the stuff.  The peroxides will be concentrated by boiling the ether and near the end of the distillation ->BOOM!!
Peroxides are created by exposing ether to air, light, and probably other stuff too.  There is a couple of ways to remove the peroxides by washing the ether with some aqueous solutions or something.  Look it up in Vogel's practical organic chem book if you are interested.   

Buzzzzz........this song rocks.........
--the hive makes the world a happier place.......

[KrZ]

Most ether you buy from a chemical supplier will be stabilized against peroxides, and if you spray ether out of a starter fluid can into a flask and go straight to distillation there won't be any peroxide problems.  However, the advice about running a tube outside for any non-condensed vapours should definitely be taken.  Just don't store ether in a jar with any headspace where it will be exposed to atmospheric oxygen, or even better, purge the headspace with nitrogen before storing.

[Lilienthal]

Add some NaOH plates to your ether, they will prevent the formation of ether peroxides and keep the solvent dry.

[foxy2]

Lili
So plain NaOH to already dry ether will prevent peroxides.
Will it dissolve?
Will it work for THF?
I'd imagine only a tiny bit is necessary for this right??
Thanks
Foxy  

Happy New Year

[Lilienthal]

It will not dissolve, use something like 50 plates per liter (not critical).

It should work for all ethers (like THF) and should also slowly destroy already built peroxides (but I have no references for that and I'm not absolutely sure about it).

[foxy2]

Hmmm
My NaOH is in little half sphere/pill shaped.
So 50 of these will do the trick?


Do Your Part To Win The War

[Lilienthal]

Si senor!

[Dr_Sister]

The sister has taken post pseudonitrosite rxn mixtures tossed em with the aqueous and etherial lyaers into 2l Rb , put on a water bath. No problems so far. Usually adda dash of EtOH afterwards as a stabilzer Ta Dah! Round n around we go. Oh yeah, we always run a hose from the receiver outside to deal with the fumes.

1st time we were all freaked out used a blast shield etc., don't bother with it anymore. Generally these are very short distillations as well.