2. Add this solution to the cooled suspension of diazotized sulhanilic acid in the beaker. Stir the mixture vigorously. In a few minutes, a red precipitate of helianthin should form. Keep the mixture cooled in an ice bath for about 15 minutes to ensure completion of the coupling
Measurement of lipid peroxidation TBARS, a measure of lipid per oxidation, was measured as described by Ohkawa . Briefly, 1 ml of suspension medium was taken from the 10% tissue homogenate. 0.5 ml of 30% Trichloroacetic acid (TCA) was added to it, followed by 0.5 ml of 0.8% thiobarbituric acid (TBA) reagent. The tubes were covered with aluminium foil and kept in shaking water bath for 30 minutes at 80°C. After 30 minutes, tubes were taken out and kept in ice-cold water for 30 minutes.
in the first step benzoic acid was reacted with excess of thionyl chloride using acetonitrile as a solvent and keeping the mixture on an ice bath for 3-4 hours (labeled as reaction mixture a) In the second step gemcitabine hydrochloride along with 3eq tri-ethyl amine and using ethanol again as a solvent was stirred for 15-20 minutes without ice-bath. next with a poisterizing tube the reaction mixture a was drop wise added to reaction mixture b yielding a third and final, reaction mixture c giving off white fumes of socl2. it is stirred for 19 hours and 15minutes at 80c and colour changes to light yellow The preparation of benzoyl chloride from benzoic acid using thionyl chloride at 0’c is an in-situ preparation procedure: FILTERATION: Evaporate reaction mixture and dissolved in hexane and then filter it. The best TLC system for filterate is ethyl acetate : hexane , 4.5:0.5 3.3.2 PROCESS 2 FIGURE 3.5ACETYL DERIVATIVE PROCEDURE In 75mg of gemzar, 2ml ethanol is added and then solubility is checked. After 5 minutes add 0.1 ml (5 drops) DMF, then add 0.104ml Et3N and add 0.036 ml acetyl chloride and stirr it for 17 hours r at 47C
Referring to Table 1, the reactants for each run were transferred to an Erlenmeyer Flask (250 mL) via a buret. Using a precision pipette, the volume of I3- required for each run was carefully extracted and poured into the flask containing all of the reactants. Immediately after the Iodine solution was placed in the flask, the LabQuest began collection data. Meanwhile, a small portion of the solution, was used to rinse the cuvette, then using a disposable pipette a small amount of the solution was transferred to the cuvette (approx. ¾).
Fifteen milliliters was transferred to a clean tube marked H, for whole homogenate, and kept on ice at all times. The remaining fifteen milliliters of homogenate was transferred to a clean centrifuge tube and placed in a beaker of crushed ice. A balance was prepared by putting fifteen milliliters of distilled water into a new centrifuge tube and both tubes were then placed into the refrigerated centrifuge. It was then centrifuged at 5000 rpm for twenty minutes. When the centrifuge stops, the tube containing the homogenate was retrieved and held at the same angle.
Approximately 2 gm, nearest to 0.1 mg, oven dried cornhusk fibres, were weighed out accurately in weighing bottle and transferred to a 100 ml beaker. 40 ml of cold (10-15˚C) 72% sulphuric acid was added gradually to the fibres in small increments while stirring the mixture and macerating the fibres with a small glass rod. The beaker was kept in a bath at 2 ± 1˚C for dispersion of material. After the specimen was dispersed, beaker was covered with a watch glass and kept in a bath at 20 ± 1˚C for 2 hours. Mixture was stirred frequently to ensure complete
Grade) in 1 l water, standardize this solution with 0.0192(N) silver nitrate solution. The solution losses strength gradually and must be rechecked every week. 1 ml of solution = 1 mg CN (ix) Standard cyanide solution: Dilute 10 ml stock cyanide solution to 1 litre with distilled water, mix and make a second dilution of 10 ml to 100 ml. Prepare fresh solution daily. 1 ml = 1 µg CN (x) Chloramine –T: Dissolve 1 gm chloramine – T in 100 ml distilled water.
Obtained product was immediately used for next step. Step-4 Synthesis of 2-Methyl-3-[5-(4-substituted)phenyl-1,3,4- oxadiazole-2-yl]- quinazoline-4(3H)-ones53 (5) To the mixture of benzoxazinone (4), 2-Amino-5-aryl -1,3,4-oxadiazole (0.1M) in 100ml of glacial acetic acid was added and refluxed under anhydrous condition for 4 hrs. After cooling it was poured into crushed ice. The solid separated out was filtered thoroughly washed with cold distilled water, dried and recrystallised from hot ethanol (95 %). 5 Table 5 : Quantity of Oxadiazoles taken for synthesis S.No.
Linoleic acid peroxidation was initiated by the addition of 4 mM FeSO4.7H2O, incubated for 60 min at 37oC and terminated by the addition of 2 mL of ice cold trichloroacetic acid (10% v/v). An amount of 1 mL of thiobarbituric acid (1% w/v in 50 mM NaOH) was added to 1 mL of the reaction mixture, followed by heating at 95oC for 60 min. The reaction sample was read at 532 nm.7 The percentage of linoleic acid peroxidation inhibition activity was calculated using the following equation: % Inhibition = [(AB - AA)/AB] x 100, where AB, absorption of blank sample, AA, absorption of test sample. 2.5.4. Metal chelating activity Briefly, 2 mM FeCl2 was added to different concentrations of test sample and reaction was initiated by the addition of 5 mM ferrozine.
During this step, I observed that there were bubbles in the solution, especially at the bottom of the beaker. After adding the HLC, there solution had a slight yellow tint. Next, I mixed 0.529g of sodium acetate in 3mL of water and added 0.679g of acetic anhydride to the aniline solution and immediately added sodium acetate. The solution was cooled in an ice bath for fifteen minutes. During this time, I noticed the formation