One-step synthesis of magnetically recyclable palladium loaded magnesium ferrite nanoparticles: application in synthesis of anticancer drug PCI-32765

Abstract

Novel Palladium nanoparticles supported nano Magnesium ferrite catalyst (Pd/MgFe₂O₄) was synthesized by one-step ultrasound assisted coprecipitation. In-situ formed by-products assisted salt cage calcination approach was employed to control the particle size by minimizing the risk of nanoparticle aggregation during calcination. Palladium nanoparticles were grafted on the surface of nanocrystalline MgFe₂O₄ without using any reducing agents, capping agents and surface modifiers. The catalyst preparation method was having minimum process operations and can be used for synthesis of various potential nanocatalytic systems. The catalyst was extensively characterized by using various techniques SEM-EDS, TEM, FT-IR, XPS, XRD, VSM, BET, and ICP-AES. Pd/MgFe₂O₄ was magnetically separable and shown its potential utility for ligand less Suzuki-Miyaura coupling reaction using green solvent system Water and Ethanol. The nanocatalyst shows consistent activity and excellent reusability in the synthesis of Biaryls with excellent yields. In addition, the prepared catalytic nanoparticles were successfully applied in the synthesis of 5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-ylamine an intermediate for preparing the marketed anticancer drug PCI-32765 under the name IMBRUVICA® (Ibrutinib-BTK inhibitor).

Keywords:

• One-step synthesis
• coprecipitation
• salt cage assisted calcination
• Pd-Magnesium ferrite
• magnetic nanoparticles
• Suzuki-Miyaura coupling

Acknowledgments

The authors are very thankful to SAIF Department IIT Bombay, India, Center for Excellence: Nanotechnology, Andhra University, Visakhapatnam, India. The authors are thankful to M/S Shilpa Medicare Limited for providing the opportunity and Dr. Sriram Rampalli, Dr. Lavkumar Upalla for continuous support and encouragement.