L. Yang et al. / Carbohydrate Research 346 (2011) 2304–2307
2307
to 1000 W, and can be averagely divided into 10 gears, which can
be automatically adjusted. The microwave reaction apparatus is an
open system. The reaction mixture was placed in round-bottom
reaction flask with a magnetic stir bar, and then a reflux condenser
was attached. The water used in the experiments was all twice-dis-
tilled water.
R = 0.999. Then, the concentration of 1-(furan-2-yl)-2-hydroxyeth-
anone in the measured solution was calculated according to this
standard equation.
Acknowledgments
This work was financially supported by the National Natural
Science Foundation of China (No. 20876032), Tianjin Key Research
Program of Application Foundation and Advanced Technology (No.
11JCZDJC23600) and Application Bases and Key Research Program
of Hebei Province (No. 11963924D). The authors would like to
thank Dr. Zhiming Fan from CanmetENERGY, Upgrading Program
of Natural Resources Canada, for his helpful instruction and lin-
guistic revision.
1.2. Conversion of cellulose into 1-(furan-2-yl)-2-
hydroxyethanone
Cellulose was dissolved in 140 mL ZnCl2 solution (ZnCl2:H2O ra-
tio = 2.25:1.00, w/w), and the above mixture was subjected to MW
at 600 W for 5 min and a reaction temperature of 135 °C. The reac-
tion mixture was extracted repeatedly with EtOAc (5 Â 50 mL), and
then the combined extracts were concentrated under vacuum. This
crude extraction included a number of furans, a small amount of
acids and other small-molecule compounds as examined by GC–
MS. The crude extract was separated and purified by column chro-
matography on silica gel (1:8 to 1:4 EtOAc–CHCl3) to give a yellow
needle-like product in a yield of 26.6%. In addition, we also isolated
5-HMF from the degradation solution, and the weight yield of the
product was 47.2%. 1H NMR and 13C NMR spectroscopy and MS
were used to characterize the products (see earlier Discussion).
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, linear correlation coefficient of