Benzoyl Hydrazone Experiment

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Experimental Methods: 1. SYNTHESIS OF 4-BENZOYL BUTYRIC ACID METHYL ESTER Materials required * 5 oxopentanoic acid : 2 gm (Aldrich) * Methanol : 50 ml * Acetic Acid (Rankem) Procedure: * 2 grams of 5 oxopentanoic acid was weighed and placed in a round bottom flask and then to it 50 ml of methanol was added. It was placed on a hot plate and the temperature was increased to 50 degrees under ambient air conditions. * To the RB, 2 ml of acetic acid was added and then by attaching a condenser the entire reaction was put on refluxing at 70 degrees Celsius in an oil bath. * For work up: * The reaction media was concentrated till about 10 ml and then dry silica gel was added. * The column was packed and while using DCM as solvent it was started.…show more content…
REACTION OF HYDRAZONE WITH C60: Synthesis of PC61BM Materials required: * Methyl-4- benzoyl butyrate p- tosyl Hydrazone – 50 mg * Dichloromethane- 7 ml * Triethylamine-0.7 ml * C60 powder – 33.6 mg * ODCB – 7 ml Procedure: * The hydrazone synthesized in the previous step was weighed for 50 mg and carefully transferred into a two neck round bottom flask which was placed in between an ice bath which was kept on a magnetic stirrer. * To the above RB, 55mg of pre hydrazone was added and placed in the above described RB which was placed on the magnetic stirrer. * To the above, about 0.7 ml of triethyl amine was added into the RB using a syringe. * Stirring was continued for about 3 hours approximately at this temperature. * At the same time, 33 mg of fullerene was dissolved in 5 ml of Orthodichloro benzoic acid. And it was stirred for about 3 hours in a separate conical flask. * With the help of a dropper the dissolved fullerene was added into the RB which had the hydrazone. * Once the addition was complete the temperature was increased to 80 degrees and it was kept on refluxing for overnight duration. * The progress of the reaction was checked from time to time by checking the TLC in the solvent of the column, that is…show more content…
TGA thermogram of mGO and PCBGO under nitrogen atmosphere. 4. RAMAN SPECTROSCOPY * For organic materials raman spectroscopy is the ultimate characterisation technique employed. * In our synthesis functionalization of Graphene sheets with PCBM molecules is clearly seen and can be evaluated. * In GO the Defect(D) peak and Graphitic(G) peak are seen at 1359 and 1586 cm-1 respectively. * Upon functionalisation there is no change in the defect peak but the G peak shows two fittings for the sp2 and sp3 hybridisation in graphene and fullerene respectively. * Also the G band is highly red shifted. * Appearance of 2D peak at 2795 cm-1 and G’peak at 2913 cm-1 due to large domain size of sp2 carbon network. * Further the ID/IG ratio of GO and PCBGO were compared to see the size of the sp2 domain in each and to compare. In PCBGO it is highly reduced in comparison to GO. Raman spectra of mGO and PCBGO excited by 515.5 nm laser beam. Dotted line shows the fitting of peaks. 5. X-RAY DIFFRACTION * XRD is a technique generally employed for elucidation of structure and arrangement of atoms. * In our analysis the structure of GO and PCBGO were

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