Author:
Bagnell Laurence,Bliese Marianne,Cablewski Teresa,Strauss Christopher R.,Tsanaktsidis John
Abstract
A moderately yielding (50±4%) method for obtaining
3-methylcyclopent-2-en-1-one from hexane-2,5-dione in ≥99·5%
purity was developed, using 2·1% (w/v) of aqueous KOH at
reflux. However, the yield was increased to 80±5% by using
considerably lower concentrations of base (<0·1%) and higher
temperature (200°C) with a conventionally heated autoclave or a microwave
batch reactor. The preparation was scaled up with a larger autoclave and also
with a continuous flow microwave reactor. The dione impurity was removed from
the enone by preferential adsorption on an anion-exchange resin in the
bisulfite form. The product was recovered from the aqueous phase with a
hydrophobic resin. This environmentally benign, non-extractive isolation
method has potential for broad applicability in cleaner production.
Cited by
43 articles.
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