2-Methylcyclohexanone Lab Report

Chloroacetic acid (0.5 g, 5. 28 mmol), 5-aminotetrazole monohydrate (0.45 g, 5. 28 mmol), and sodium hydroxide (0.59 g, 10.57 mmol) in 10 ml of water was refluxed 20 hr, cooled, and made strongly acidic with concentrated hydrochloric acid. The mixture was cooled overnight and precipitate was separated to give 0.28 g a white solid product at 45.41% yield. (5-Amino-tetrazol-1-yl)-acetic acid: Yield: 45.41%; white crystals; m.p 210-213°C; IR (KBr): 3388, 3315, 3270, 3205, 3010, 2976, 1697, 1638, 1586, 1496, 1257 cm-1; 13C NMR (75 MHz (DMSO-d6)): 168, 156,

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.

We also used ice to see whether unknown compound will dissolve in the ice. We used 3ml of ice and 0.5 g of unknown and 1-gram sodium carbonate and 1g unknown carbonate in 10 ml H20. when we first mixed ice with unknown it melts then we used sodium carbonate and unknown carbonate it forms white precipitate. for the final test we used 1-gram sodium bicarbonate and unknown with 15 ml of H20 then it bubbles up. After we done with all other test, we like to see the PH of the sodium bicarbonate and unknown, its initial temperature is 20 and the final temperature was 24 and then PH paper turn blue and its has the PH of 8-9 and its very

2.3. Synthesis of 2-(2-(Morpholinomethyl)-1H-benzimidazol-1-yl)acetohydrazide (4) To a solution of compound 3 (0.01 M, 2.89 g) in methanol (60 mL), 99% hydrazine hydrate (1 mL) was added and the mixture was refluxed for 6 h. The reaction mixture was cooled and the solid thus obtained was filtered, washed with cold water and recrystallized with ethanol to obtain the compound 4. 2.4. General procedure for synthesis of 1-{(5-substituted-1,3,4-oxadiazol-2-yl)methyl}-2-(morpholinomethyl)-1H-benzimidazoles (5a-r) An equimolar mixture of compound 4 (0.001 M) and substituted carboxylic acid in phosphoryl chloride (POCl3) was refluxed for 8–12 h. Then reaction mixture was cooled, poured into ice-cold water and neutralized with 20% w/v NaHCO3 solution.

Production diclofenac acid (DFA) by diclofenac sodium (DFS) hydrolysis DFA which yielded from DFS hydrolysis was characterized by FT-IR and DTA. Fig. 2 showed the information provided by the spectra FT-IR profile, which distinguished DFS from DFA. The DFA’s spectra showed a specific absorption peak at 3324 cm-1 which correspond to free OH stretching of a carboxylic group. Free acid was also presented as a peak at 1693 cm-1 associated with C=O stretch and 1157 cm-1 correspond to the C-O stretch.

Figure 1 shows the synthesized ionic liquid of CVD with studied acidic compounds (white crystalline materials) in 1:1 molar ratio after dissolving them in methanol and complete solvent evaporation after five days. CVD with CA, TA and SAC convert to a viscous yellow liquid form. This method was used to preparation of different ionic liquid form of drugs such as ketoconazole with TA and CA (24) and sulfasalazine and acyclovir with choline (28). ****Fig 1**** The DSC thermograms of CVD, CA, TA and their ionic liquid forms have been demonstrated in Figure 2. They shows that CVD and studied acidic compounds are crystalline and they have a distinct endothermic peaks corresponding to the melting of solid forms.

MDA level was determined by thiobarbituric acid reactive substances (TBARS) in serum, based on the reaction between MDA and TBARS. Standard Malondialdehyde solution in 5 mL of volume was processed along with test samples. 1.5 mL of 0.8% of TBA was added to 1 mL of the serum sample. Then 0.4 mL of 8.1% sodium dodecyl sulphate and 1.5 mL of acetic acid was added. The mixture was finally made upto 5 mL with distilled water and placed in hot water bath at 95ºC for 1 h. After cooling, 1 mL of distilled water and 5 mL of the mixture of n-butanol and pyridine (15:1, v/v) was added.

This was repeated until no more gas was released. Next, the funnel was suspended through a ring, and 10 ml of 5% sodium hydroxide was added. When the two layers were separated in the separatory funnel, the aqueous layer was identified. The two layers were then separated into two different beakers. The water layer was acidified by adding concentrated hydrochloric

The volumetric flask was then filled up to its 100 mL mark with deionized water. The buret was washed out with dionized water and then with the strong base NaOH before being filled up with NaOH. About 20 mL of the unknown weak acid was pipetted into a beaker. The starting volume of the NaOH in the buret was recorded before about 4 mL of the strong base was titrated into the weak acid solution. The final volume was recorded.

The aqueous extract was prepared by dissolving 1g of dry extract with 20 ml of sterilized distilled water, so the final concentration of extract would be 0.05 g/ml, from this solution other concentration were prepared (0.1-0.2) g/ml. the solutions were shaken for 30 min. The extract was centrifuged (30,000 rpm; 15 min) and the supernatant was Separated. To hydroalcoholic extract, 80 g of the powder was extracted with aqueous methanol (75%). The other two concentrations were prepared from soaking sixfold aqueous methanol (75%) with different amounts of powder.