1-Butanol → Butyl oxoacetate

Participants

Reaction Conditions

Reaction Steps

300 g of 1-butanol was added to 60 g of a 40 wt % glyoxal aqueous solution (Wako Pure Chemical), and most of the water was distilled off as an azeotropic composition with the 1-butanol at normal pressure and 90° C. with an evaporator. This gave a butanol solution of glyoxal (containing 19.4 wt % glyoxal and 80.6 wt % butanol). 5.17 g of the above-mentioned butanol solution, 8.90 g of 1-butanol, and 0.6 g of the above-mentioned metal-loading carrier were then put into an autoclave equipped with a condenser, the system was maintained at an internal pressure of 0.5 MPa at 80° C. under stirring while a mixed gas of hydrogen and nitrogen (hydrogen:nitrogen=1:9 (volumetric ratio)) was bubbled into the solution at a flux of 500 mL/minute, and the reaction was allowed to continue for 5 hours. After the reaction, the reaction solution was analyzed, which revealed the glyoxal conversion to be 87%, and the 1-butyl glyoxylate (the product) selectivity and yield to be 73% and 64%, respectively.

Provenance & Evidence