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With perrhenic acid anhydride; at 320℃; for 6h;Inert atmosphere; Sealed tube;
General procedure: The catalytic reactions were carried out in a batch reactor (ParrInstruments, 300 mL). In a typical model compound conversion experiment,the reactor was loaded with 0.1 g catalyst, 1 g substrate,60 mL solvent, sealed and purged with N2 five times. The reactor wasthen heated to the desired reaction temperature within 1.5 h and kept atthis temperature for the desired reaction time with stirring at 550 rpm.The reaction time was denoted as 0 h when the prescribed reactiontemperature was reached. After the reaction, the reactor was firstlycooled in air by removing the heating jacket. On reaching below 150 C,the reactor was further cooled by immersing it into cold-water. Thepost-reaction solution and the spent catalyst were separated by filtration.The solution mixture was analyzed with an Agilent Technologies6890 N gas chromatograph (GC) equipped with a HP-5 MS capillarycolumn (Agilent, 30m ×0.25mm ×0.25 mum) and a FID detector withanisole as the internal standard. However, when the substrate was anisole,tridecane was chosen as the internal standard. The GC parameterswere: inlet temperature 280 C, detector temperature 300 C, split ratio1:50. The oven temperature ramped from 45 C to 105 C at 15 Cmin-1, and then ramped to 280 C at 6 C min-1. Products wereidentified with a gas chromatograph-mass spectroscopy (GC-MS,Agilent Technologies, model 5973). The mass spectrum acquired withthe GC-MS was retrieved in the NIST Mass Spectral Library to identifythe structure of each product.
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