Ketones Lab Report

1. Introduction

Friedel–Crafts acylation of aromatic compounds is one of the most important and practical methods to prepare aromatic ketones. The resulting diaryl ketones are important chemical intermediates for the synthesis of a wide range of compounds such as pharmaceuticals, fragrances, flavors, dyes and agrochemicals [1,2]. This is an electrophilic acylation of aromatic compounds with acid chlorides or acid anhydrides, which is traditionally catalyzed by Lewis acids, such as AlCl3, BF3, SbCl5, FeCl3, ZnCl2, SnCl4, TiCl4 or strong protonic acids, such as H2SO4, HF [3-7]. The major drawbacks of these catalysts are that they are hazardous, corrosive, non-recoverable and usually more than stoichiometric amounts of catalysts are required.

ZPFe (3 mol%) was added to a mixture of a benzoyl chloride (10 mmoL) and an aromatic compound (10 mmoL). The reaction mixture was stirred for the appropriate reaction times at 80 °C (Table 2). After completion of the reaction (monitored by thin-layer chromatography, TLC), the mixture was diluted with Et2O and filtered. The organic layer was washed with 10% NaHCO3 solution and then dried over anhydrous Na2SO4. The solvent was evaporated under reduced pressure and the product purified by column chromatography on silica gel to give the corresponding pure aryl

2). The SEM micrograph of ZP, Fig. 2a., shows the hexagonal plates that the disks had well-defined shapes with very smooth surface. Fig. 2b. shows the SEM image of ZPFe which is much less ordered in comparison to that of ZP. It shows some aggregation of ZPFe particles in both sheets and spherical shapes, where its particles are mostly conglomerate with uneven shape and size. Fig. 3 represents the TEM (CENTRA 100, Zeiss) images of ZP and ZPFe. The TEM images of ZPFe, Fig 3a and 3b (different magnification), show that the ZPFe retains the original morphology of the ZP, and a size of ~ 150 nm with clear crystal habit was observed. They show nanoparticles, which are on the smooth surface of the ZP with different sizes. The observable existence of metallic crystal nanoparticle indicates that agglomeration of iron deposited on the surface of the ZP. Almost the same observations were reported for zinc and cerium zirconium phosphate earlier [34,