Table 6. Effect of Reaction Temperature on HMF Conversion and DFF Yield in CH3CNa.
entry | temperature (°C) | conv. HMF (%) | yield DFF (%) | select.b (%) |
---|---|---|---|---|
1 | RT | 16 | 15 | 94 |
2 | 30 | 57 | 55 | 96 |
3 | 40 | 72 | 69 | 95 |
4 | 50 | 100 | 94 | 94 |
5 | 60 | 54 | 52 | 96 |
6 | 70 | 28 | 27 | 96 |
Reaction conditions: HMF (1 mmol, 126 mg); Fe(NO3)3·9H2O (0.05 mmol), TEMPO (0.05 mmol, 7.8 mg), NaNO2 (0.05 mmol, 3.4 mg), CH3CN (5 mL), and oxygen balloon; the conversion and yield were determined by HPLC. Conv. = conversion. Select. = selectivity.
S (DFF) = yield (DFF)/conversion (HMF).