In the study, the epoxidation process
of soybean oil by microflow
system (MFS) was investigated. With formic acid as oxygen carrier
and EDTA-2Na as stabilizer, the optimal result (epoxidized soybean
oil (ESO) with an epoxy number (EN) of 7.3) was obtained in such conditions:
temperature 75 °C, H2SO4 concentration
3%, EDTA-2Na dosage 3%, residence time 6.7 min, ratio of formic acid
to hydrogen peroxide 1:1, and H2O2 to double
bond molar ratio 8:1.
4-Nitropyridine, a key intermediate in medicinal products, was successfully prepared from pyridine N-oxide in a two-step -approach. Pyridine N-oxide was nitrated with HNO3 and H2SO4 to give 4-nitropyridine N-oxide, followed by reaction with PCl3 to give the final product. The continuous flow methodology was used to minimise accumulation of the highly energetic and potentially explosive nitration product to enable the safe scale-up of 4-nitropyridine with no 2-nitropyridine by-product. By employing continuous extraction in the nitration step and applying the optimised conditions, a throughput of 0.716 kg 4-nitropyridine product per day from pyridine N-oxide with 83% yield and high selectivity in a continuous flow system was achieved.
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