Microwave Oven Reaction Enhanced (MORE) Chemistry

Pressure vessels (release valves not shown)
Since the mid 1980's, we have experimented with numerous reactions to see whether they can be performed more efficiently in conventional microwave ovens.
A number of these have given significant reduction in heating times without any appreciable loss of yield or purity.
For example, see the preparation of Cr(acac)3 in the C 21J Laboratory Manual.
We have used 60 and 120 mL Teflon vessels purchased from:
Savillex Corporation,
    6133 Baker Road,
    Minnetonka, 
    Minnesota, 55345-5910
    USA
    Tel (952) 935-4100
    Fax (952) 936-2292

this is not a commercial, but, compared to other brands we have tried, only a few have exploded on us over the years!!
In their Catalog #15, 1994 page 27, they quote prices of:

  $ 91.20 for 4 of the 60 mL vessels (#561R2)
  $167.20 for 4 of the 60 mL vessels (#568) with pressure relief valves,

  $121.60 for 4 of the 120 mL vessels (#571R2).
  $193.80 for 4 of the 120 mL vessels (#578) with pressure relief valves.
In general, students are warned not to fill to more than about 10% of the volume of the container so as to allow a fairly large head-space.

In the Chromium preparation mentioned above, the conventional heating time is over three hours, whereas in the microwave oven, the product precipitates in the Teflon vessel in under ten minutes.

See our paper on the preparation of substituted stilbenediamines presented at ECTOC in 1995.

For further details see:
H.M. Kingston and L.B. Jassie, "Introduction to Microwave Sample Preparation- Theory and Practice", American Chemical Society, Washington D.C., USA, 1988.
D.R Baghurst, D. Michael and D.M.P. Mingos, Chem. Soc. Rev., 1991,20, 1-47.

and look at the Duquesne University WWW site on the use of Microwave Ovens in sample preparation.
On the CEM web site you can find details of their MARSX equipment for solvent extraction at elevated temperatures and pressures as well as Carboflon(R) inserts for heating non-polar solvents.

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Created and maintained by Prof. Robert J. Lancashire,
The Department of Chemistry, University of the West Indies,
Mona Campus, Kingston 7, Jamaica.
Created Feb 1995. Links checked and/or last modified 24th August 2004.
URL http://wwwchem.uwimona.edu.jm/lab_manuals/MORE.html