A novel method for
the synthesis of triphenyl
phosphite and its derivatives has been developed in continuous flow.
With a total residence time of 20 s, the target product was prepared
in a microreactor, and the reaction time was significantly shortened
compared with standard single batch reaction conditions. In addition,
the reaction of various substrates gave the corresponding products
in good to excellent yields under optimized conditions. The reactants
could be employed in a stoichiometric ratio, making the reaction more
efficient, economical, and environmentally friendly. In addition,
scale-up apparatus was designed and assembled, and the kilogram-scale
production (up to 18.4 kg/h) of tris(2,4-di-tert-butylphenyl)
phosphite was achieved in 88% yield.
A practical approach to the synthesis of antioxidant 4,4′-dicumyldiphenylamine (DCDPA) and its derivatives by Friedel−Crafts alkylation of aromatic amines was developed under continuous flow conditions. Because of the enhanced mass and heat transfer features of the microreactor, the reaction time was significantly reduced in contrast to a batch mode. The reaction was carried out using a 1:6 v/v ethanol/Cl(CH 2 ) 2 Cl cosolvent system with ZnCl 2 as the catalyst to achieve satisfactory yields. This is an effective method for the synthesis of DCDPA and its derivatives with excellent para selectivity that has the merits of shorter reaction time, easy operation, and straightforward scale-up.
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