Table 3. Scale-Up HMF Reactions in an Autoclavea.
selectivity %b |
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D-fruct. g | DMC mL | crude HMF g | HMF | OBMF | HMF yield %b | HMF crystals yield % | HMF-rich oil g | BHMF yield %c | total yield %d |
10 | 40 | 5.37 | 98 | 2 | 73 | 47 | 1.86 | 75 (18) | 65 |
20 | 80 | 11.21 | 98 | 2 | 76 | 44 | 4.61 | 78 (21) | 65 |
30 | 120 | 17.08 | 97 | 2 | 77 | 45 | 6.72 | 70 (19) | 64 |
40 | 160 | 22.76 | 96 | 4 | 72 | 46 | 7.92 | 73 (17) | 63 |
Reaction conditions: d-fructose was dissolved in DMC/TEAB in the presence of Purolite CT275DR (5% wt.) at 110 °C in an autoclave for 2 h.
Evaluated via 1H-NMR spectroscopy.
Isolated yield calculated with respect to the HMF contained in the residual oil; in parenthesis, yield calculated with respect to the starting amount of d-fructose.
Considered as HMF crystals + HMF converted into BHMF.