Nickel exchanged supported 12-tungstophosphoric acid: synthesis, characterization and base free one-pot oxidative esterification of aldehyde and alcohol

2019 
The present work describes for the first time, the synthesis and characterization of a bi-functional catalyst consisting of nickel and supported 12-tungstophosphoric acid as well as its application in one pot oxidative esterification of benzaldehyde and benzyl alcohol to benzoate ester. The said reactions were operated without any base at a low temperature and atmospheric pressure. The influence of reaction parameters such as nickel concentration, molar ratio of substrate to H2O2 as well as methanol, catalyst amount, reaction temperature and reaction time were investigated to optimize the conditions for maximum conversion with good selectivity towards the desired product. The superiority of the present work lies in obtaining higher conversion as well as higher selectivity of the desired product with a high TON for both the systems under sustainable reaction conditions. Moreover, the catalyst could be recovered and reused for up to three cycles without any significant loss in its selectivity. The obtained conversion as well as selectivity were discussed with a number of control experiments and based on the obtained results, mechanisms for both the reactions were proposed. Furthermore, the difference in activity towards oxidative esterification of benzaldehyde and benzyl alcohol was also correlated with the proposed mechanism.
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