Add 10-12 mL glacial acetic acid gradually, so as to precipitate the anthranilic acid . Filter the separated acid, wash with cold water and recrystallize it from hot water. Mechanism: Step III: Preparation of o-chlorobenzoic acid from anthranilic
The nanoparticles of Zinc oxide at 10 wt% were added in the above solution with vigorous stirring in order to get the homogeneously suspended Zinc oxide nanoparticles in the solution. Further slowly added 0.1 M of ammonium persulphate drop-wise which acts as an oxidizer with continuous stirring to this solution. The temperature was maintained at 4oC by keeping in the ice for 4 hours for polymerizing completely. Then the precipitate was filtered, washed with deionized water, acetone and finally dried in an hot air oven for 24 hours. Similarly PANI/ZnO Nanocomposites at different weigh percentages, that is 20%, 30%, 40% and 50 wt% could be synthesized.
The mentioned ratio of the two materials were collected in a quartz crucible. Next, de-ionized water was added into the quartz crucible containing the nickel nitrate and urea. The de-ionized water was poured until it made up 50% of the portion of the solution After that, the entire solution was placed in an oven for about 1 hour. This was done to age the mixture and the temperature was maintained at 80oC. The solution was then taken out of the oven to be put in a pre-heated muffle furnace which was maintained at 650oC.
Synthesis of 3-[5-(4-substituted) phenyl-1,3,4-oxadiazole-2yl]-2-styrylquinazoline-4(3H)-ones was carried out by following steps: Step 1: Synthesis of 4- substituted benzaldehyde semicarbazon51(2) Semicarbazide Hydrochloride (0.1M) and sodium acetate (0.2M) was added and dissolved in 15-20ml of distilled water placed in flat-bottomed flask. In a separate beaker containing required aromatic aldehyde (1) (0.1M) was dissolved in aldehyde free alcohol. This ethanolic aromatic aldehyde solution was added slowly to the solution of semicarbazide hydrochloride. The precipitate, which gets separated, was filtered, dried and recrystallised from 95% hot ethanol. Table 1: Quantity of aldehydes taken S. No.
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 N‟-2- (bromophenyl)-N,N-dimethylurea 16 underwent lithiation on the nitrogen to form a monolithio intermediate using MeLi, followed by bromine-lithium exchange using t-BuLi to give the dilithio species 17. 14 The intermediate 17 was then exposed to carbon monoxide to give 18, which after cyclization forms the intermediate 19, followed by loss of LiNMe2 to give 20, and finally after work up with dilute acid yielded the isatin product 1. 1 13 14 15 6 N O O 1) MeLi, 0 C CO Br N H O NMe2 2) t-BuLi, 0 C Li N O NMe2 Li C N Li O Li O NMe2 N O NMe2 O Li Li -LiNMe2 N H O O Li H3O + X X X X X X A rather versatile and novel two step synthesis of isatins was presented by Mironov in 2001 and allowed for the preparation of isatins containing electron withdrawing groups such as - CF3, -NO2, and -Cl. The method is based on the reaction between aromatic isocyanides and tertiary amines,15 where in the first step, 2-triethylammonio-3-arylaminoindolates 23 were obtained from the corresponding aromatic formamides 21 without isolation of the intermediate isocyanides 22. 16 Heating the 2-triethylammonio-3-arylaminoindolates 23 in excess thionyl chloride followed by hydrolysis led to the target
The volume was made with 6.8 pH Phosphate buffer to get a concentration of 1000µg/ml (SS-I). UV Absorption Maxima (λ max) of Itraconazole sample in pH 6.8 Phosphate buffer • Stock II: 10ml of above solution was then further diluted to 100ml with 6.8 pH Phosphate buffer to get a stock solution of 100µg/ml. UV scanning was done for 100 µg/ml drug solution from 200-400 nm using pH 6.8 Phosphate buffer as a blank in Shimadzu, UV 2450 spectrophotometer. The wavelength maximum was found to be at 262
Results and discussion Reaction mechanism of the sol-gel process Monodisperse silica NPs can be prepared by hydrolysis and condensation of alkoxysilanes in a mixture containing alcohol, water, and catalyst. The chemical reactions describing the hydrolysis and condensation of TEOS and MTES are shown in Fig. 3. As shown in this figure, TEOS can be hydrolyzed and condensed to form SiO2 colloid particles in mixture of Methanol, NH4OH and H2O after being stirred for 1 h at room temperature. Similar to the results reported by Wang et al., the obtained inorganic silica (SiO2) colloid particles have active hydroxyl groups on their surfaces.
Experimental Procedure Materials: Egg shells, Orthophosphoric acid(99%SIGMA ALDRICH), Titanium dioxide (99%SIGMA ALDRICH),Ammonia solution. Pure Hydroxyapatite synthesis: Cleaned and Uncrushed eggshells were calcined in air atmosphere at 900 ºC for 1h, organic materials will decay during heating of first 30 minutes, later on the egg shells will be recovered as calcium oxide. Then the calcined eggshells are grinded into very fine powder using mortar. 5gms of egg shell powder were dispersed in distilled water.To this2M of Ortho phosphoric acid is added drop by drop with continuous stirring for 1hr such that Ca /P ratio is 1:67.The pH is found to be 8.5 at the end of the reaction. The precipitate formed was subjected to aging treatment for
2 ml, 3 ml, 4 ml, and 5 ml solution was withdrawn and same procedure was repeated as above. Solutions were diluted to get concentration of 10 μg/ml, 20 μg/ml, 30 μg/ml, 40 μg/ml and 50 μg/ml neomycin sulphate respectively and scanned under the UV-VIS spectra were recorded between 400-800 nm. Absorbance was measured at 566nm. Similar procedure was used for the measurement of the drug content.