Direct oxidative amidation of aromatic aldehydes using aqueous hydrogen peroxide in continuous flow microreactor systems

Xiaoying Liu, Klavs F. Jensen
2012 Green Chemistry  
All the reactions were carried out in a continuous flow system using a spiral-channel silicon-Pyrex microreactor with a total volume of 230 μL. The general experimental procedure is as follows. Two reactant solutions loaded in separate 2.5 mL syringes (Hamilton, GasTight) were delivered into the microreactor through the two inlet ports via Teflon tubings (Upchurch, 0.02 in. i.d.) with the same infusion rate that is controlled by a syringe pump (Harvard Apparatus, 9801781). Typically, one
more » ... pically, one solution contained aldehyde (1 mol/L), aqueous hydrogen peroxide (1.2 mol/L), p-xylene as the internal standard (0.5 mol/L), and acetonitrile (or tert-butanol), and the other contained amine and acetonitrile (or tert-butanol), the concentration of amine being varied for reaction optimization. The residence time control (10-100 min) was achieved by varying the flow rate of the reactants. The temperature of the reaction zone (60-140 o C) was monitored using a K-type thermocouple that was inserted into a small hole on the side of the packaging chuck and
doi:10.1039/c2gc35078e fatcat:lp7y4gjg25b3pc7ut7x2t6tevu