Oxopentanoic Acid Synthesis Lab Report

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.

2. FORMATION OF HYDRAZONE FROM ESTER
Materials required:
* The ester which was synthesized in the previous reaction. The total weight of ester obtained was 230mg.
* Methanol – 20 ml
* P-toluene sulfonylhydrazide (1.2 equivalent )
Procedure:
* The ester was transferred in a round bottom flask and it was mixed with about 20ml of methanol and stirring was done on a magnetic stirrer till the ester dissolves in it completely.
* In the above RB, a calculated amount of 1.2 equivalent amount of PTSH was added during continous stirring.
* To the RB a condenser was attached and it was put on refluxing for a time period of 18 hours at a temperature of 80 degrees in an oil bath.
* Post refluxing, the condenser was removed and it was left undisturbed for 1 day and then cooled to a temperature of -20 degrees by keeping in the freezer for setting of hydrazone crystals.
* Once the crystals were formed, the supernatant was decanted and the crystals were transferred to a beaker where they were washed with cold methanol and then dried.
* These dried hydrazone crystals were used in the subsequent steps.
3. REACTION OF HYDRAZONE WITH C60: Synthesis of PC61BM
Materials

* 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 analysed.
* The interlayer distance upon functionalisation can be seen as a function of oxidation.
* The d spacing for GO= 7.82 Å from diffraction peak at 11.4 degrees for the [001] plane.
* The d spacing for PCBGO= 10.9 Å corresponding to diffraction peak at 8.1 degrees for the [001]