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phosphoric acid (0.40 mL, 85%). The mixture was stirred until
the liquids homogenized, then left to gel. The gel was aged for
2–3 weeks before use.
Dehydration of rac-1-phenylethanol by an acidic gel
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The dehydration was performed under 1 atm N2, filtrations and
work-up were performed in air. Acidic gel (0.0433 g), prepared
as above but omitting Novozym® 435, was heated with anhy-
drous toluene (2 mL) and rac-1-phenyl ethanol (0.67 mL,
5.6 mmol) without stirring, heating oil temperature 105 °C, for
2 h. The solution was filtered from the gel under gravity and a
sample taken for 1H NMR analysis. The solution was returned to
the heat for a further 2 h and another sample taken and analyzed
1
by H NMR. The gel and solution were recombined and heated
for a final 2 h and then a final 1H NMR sample was analysed.
Acknowledgements
Thanks to Shifang Liu (CCM research), Peter Goodrich, QUILL,
ASEP (QUB) and the European Social Fund.
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