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
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.
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
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.
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.
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.
10. The solution was then placed under the fume hood for the chloroform to evaporate. 11. Methanol was filled in a test tube and placed into a water bath to heat up. 12
Then, the pipet was rinsed with distilled water. The bulbs were then attached to the pipette; filling and dispensing water were practiced using both bulbs. Furthermore, the 250-mL beaker was weighed, and its mass was recorded. After that, the Erlenmeyer flask was filled with 100 mL of distilled water. The temperature was recorded.
When determining the solubility of malonic acid in different solvents both water and methyl alcohol were found to be polar when mixed with malonic acid. Hexane however was insoluble. Lastly biphenyl was mixed with water and was found to be insoluble, methyl alcohol was determined to be partially soluble. Hexane on the other hand was the only soluble solvent for biphenyl 2. Part B. of this experiment determined the solubility of different alcohols in hexane or water.
Purpose The purpose of this experiment was to evaluate the stoichiometric relationship between the testing agents and to identify the products formed. The relationship was found by completing three acid and base neutralization reactions using phosphoric acid, which is a triprotic acid, with different volumes of sodium hydroxide. Introduction Procedure Phosphoric acid solution with a volume of 1.00 mL and a molarity of 6.00 M was transferred into a 125-mL Erlenmeyer flask using a volumetric pipette.
Observations The purpose of this experiment was to be able to synthesize triphenylmethyl bromide from triphenylmethanol by a trityl carbocation intermediate. During the experiment, 0.100 g of triphenylmethanol was placed into a small test tube. The triphenylmethanol looked like a white powder. Next 2 mL of acetic acid was added to the test tube and the solution turned a cloudy white color.