A microstructured mesh contactor that can offer residence time of more than minutes is used for gas-liquid-solid hydrogenations and gas-liquid asymmetric hydrogenations. Applications for catalyst/chiral inductor screening and for kinetic data acquisition are demonstrated.
Ozonolysis of acetic acid 1-vinyl-hexyl ester was carried out in a falling film microreactor in a continuous fashion. The influence of reaction variables (e.g., olefin concentration, ozone initial partial pressure, gas velocity, temperature and liquid flow rate) on the product formation in the liquid phase was studied over a wide range of operating conditions. Based on the obtained results, a formal reaction scheme for the ozonolysis of acetic acid 1-vinyl-hexyl ester is suggested. The acetic acid 1-formyl-hexyl ester and the corresponding carbonyl oxide are the main products of the cleavage of the primary formed ozonide. The secondary ozonide acetic acid 1-[1,2,4]trioxolan-3-yl-hexyl ester is formed by consecutive reaction of the acetic acid 1-formyl-hexyl ester and the carbonyl oxide.
A new concept for the high-throughput screening of multiphase reactions involving molecular catalysts is described. It combines pulse injections of catalysts and substrate and mixing in a microdevice. The novelty of the concept resides in dynamic sequential vs. batchwise operations. Some advantages over traditional batch parallel operations are lower inventory of sample (down to~g) coupled with accurate control of reaction time, larger range of operating conditions (pressure, temperature), simpler and fewer electromechanical moving parts and easy automation. Results on liquid-liquid (biphasic allylic alcohol isomerization), and gas-liquid (asymmetric hydrogenation) reactions indicates that the number of tests per day can easily reach 50 d-1 with inventory of sample (Rh) per test as low as 5~g.
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