Re: ORGLIST: AlCl3 purification/sublimation and drying of CS2

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From: Herb Hedgecock (h.hedgec$##$morehead-st.edu)
Date: Tue Oct 27 1998 - 10:10:14 EST


On Tue, 27 Oct 1998, Christopher Whicker wrote:

> I would be very grateful if anybody could direct me to a method for the
> purification/ sublimation of aluminum chloride, as I have a bottle that was
> old but unopened and am concerned regarding the condition of the contents.

You mention Vogel's text. It says to vacuum sublime the aluminum chloride,
use a gentle flame, connect to the receiving flask with a vacuum bend, and
with a calcium chloride drying tower connected to the vacuum,
and probably is best to not use a vacuum pump due to corrosion.

Old, unopened bottles are usually good enough for most purposes. The
rule we usually used was that if it fumed when opened to air, then it
was alright to use (at least as a Friedel-Crafts catalyst.
>
> In addition I wish to dry some carbon disulphide and have the Vogel's
> method that uses KMnO4, Hg and HgCl2, however, the method is a bit vague as
> to the amounts of each per litre of solvent to be dried (CS2).

The procedure in Vogel that you mention, is for purification of CS2. If
all you want is drying, then use calcium chloride and distill with a bath
not higher than 65 deg C.

Another suggestion is to look in Fieser & Fieser's "Reagents for Organic
Synthesis" for purification processes. I don't have them at hand, but
they are good sources for such.

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