4.1 General Remarks: Most of the reactions were carried out in oven dried glass wares with magnetic stirrer and and reflux condenser using freshly solvents. Reactions are monitored on aluminium coated thin layer chromatography (TLC) with UV light and iodine as developing agents. Melting points were determined on melting point apparatus. Proton magnetic spectra were recorded on Brucker 400MHz spectrometers using tetramethylsilane (TMS) as internal standard. Chemical shifts has been expressed in δ values downfield from TMS, multiplicity of NMR signal is designated as s (singlet), d (doublet), t (triplet), q (quartet), m (multiplet).Infrared spectra were recorded on Agilent Technologies FT-IR spectrophotometer. All solvents and reagents were purified …show more content…
Ltd. 4 Melting point Sentwin India 5 NMR Bruker Advance II 400MHz 7 Heating Mantle Inco 6 Structure builder Chem draw Ultra 8.0 4.2 Experimental work: 4.2.1 General procedure for Chalcones: 2’-hydroxy acetophenone or 2’-hydroxy propiophenone (0.2ml) and substituted benzaldehydes (0.5 g) were mixed in the round bottom flask. After that 40% NaOH solution (4g NaOH in 10 ml of distilled water) and ethanol were added in round bottom flask. The reaction mixture was stirred upto 6-48 hours. Completion of reaction was monitored in TLC plate (n-Hexane: Ethyl acetate 9:1). The reaction mixture was poured into ice cold water acidify with 1% HCl and precipitates were collected, filtered and dried and recrystalized with ethanol. 4.2.2 General procedure for synthesis of flavones: 50mg of chalcone was taken in round bottom flask. After that 15-20 ml of DMSO was added and mixed properly, 5-6 granules of iodine were added and reflux the reaction mixture up to 3-6 hours and kept for overnight. Then reaction mixture was poured into ice water and the precipitates were neutralized with sodium thiosulphate, to remove the unreacted iodine, washed with water, filtered, dried and recrystalized with …show more content…
In vitro susceptibility tests are done by the following methods: 1) Agar diffusion method 2) Tube dilution method 3) Micro-dilution method 4.3.2 Protocol: Synthesized compounds were assessed for their antibacterial activity using Agar diffusion method. Antibacterial activity of the compounds was carried out against pathogenic bacterial strains namely E.Coli: ATCC 50992 (Gram-ve), Staphylococcus aureus: ATCC 29213 (Gram+ve), Pseudomonas aureginosa: ATCC 27853 (Gram+ve), Bacillus subtilis: ATCC 10231(Gram- ve). The antibacterial activity of the compounds was determined by observing the zone of inhibition in the comparison to standard antibiotic Ciprofloxacin. Test compounds were dissolved in the DMSO to make a stock solution of 1000 ppm (1mg dissolved in 1ml DMSO). The fresh subculture of strains in the normal saline was added to the sterile assay medium (Nutrient agar) at 40-45°C and mixed well. The medium was poured in to each of the petridishes. Sterile discs of diameter 6mm were
After lawn inoculating a Meuller Hinton plate and placing the samples of medication, the plate was then incubated for one week at 37 degrees Celsius. The first medication choice was Trimethoprim, this produced a zone of inhibition of 16mm, therefore being sensitive to the bacteria. Antibiotic number two was nalidixic acid, this too, has a zone of inhibition of 16mm but is considered intermediate. The next antibiotic was erythromycin which produced a zone of inhibition of zero and was therefore resistant. The last antibiotic that was chosen to be used in the experiment was ciprofloxacin.
After 28 minutes, the mixture stopped boiling, and approximately 4.5 ml of bromobenzene was added drop by drop in the mixture, and color of the mixture was turned light brown orange. Then, the phenylmagnesium bromide was cooled in ice bath for a few minutes, and 10 ml of anhydrous diethyl ether was added in the mixture by using the syringe. After that, approximately 2.3 ml of methyl benzoate was added to the reaction, and it was added slowly slowly because the reaction was exothermic which needed to be cool in order to maintain a gentle reflux. Once all the methyl benzoate solution was added, the heating mantle was removed from the reaction flask and was cooled to the room temperature. During the reaction, a milky white salt began to precipitate, and the reaction flask was swirled for ten minutes until most of the reaction became visibly subdivided.
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.
Dalia El-Desoky Organic Chemistry II Lab 05 8 February 2017 Dehydration of 2-methylcyclohexanol Introduction: Dehydration is a common reaction in Organic Chemistry used to produce carbon-carbon double bonds. The dehydration mechanism involves the removal of water from an alcohol to form an alkene. In this experiment, 2-methylcyclohexanol will undergo acid catalyzed dehydration in heat to form three products: 1-methylcyclohexene, 3-methylcyclohexene, and methylenecyclohexane [1]. The reaction is carried out in a Hickman still filled with Drierite, a drying agent composed of CaSO4 which absorbs water.
The goal of the experiment is to synthesize a bromohexane compound from 1-hexene and HBr(aq) under reflux conditions and use the silver nitrate and sodium iodide tests to determine if the product is a primary or secondary hydrocarbon. The heterogeneous reaction mixture contains 1-hexene, 48% HBr(aq), and tetrabutylammonium bromide and was heated to under reflux conditions. Heating under reflux means that the reaction mixture is heated at its boiling point so that the reaction can proceed at a faster rate. The attached reflux condenser allows volatile substances to return to the reaction flask so that no material is lost. Since alkenes are immiscible with concentrated HBr, tetrabutylammonium bromide is used as a phase-transfer catalyst.
Benzyne Formation and the Diels-Alder Reaction Preparation of 1,2,3,4 Tetraphenylnaphthalene Aubree Edwards Purpose: 1,2,3,4-tetraphenylnaphthalene is prepared by first producing benzyne via the unstable diazonium salt. Then tetraphenylcyclopentadienone and benzyne undergo a diels-alder reaction to create 1,2,3,4-tetraphenylnaphthalene. Reactions: Procedure: The reaction mixture was created. Tetraphenylcyclopentadienone (0.1197g, 0.3113 mmol) a black solid powder, anthranilic acid ( 0.0482g, 0.3516 mmol) a yellowish sand, and 1,2-dimethoxyethane (1.2 ml) was added to a 5-ml conical vial.
The product obtained was (2S, 3R)-2, 3-dibromo-3-phenylpropanoic acid and (2R, 3S)-2, 3-dibromo-3-phenylpropanoic acid, which are enantiomers. This was determined through melting point analysis. The melting point range for the product was 198 to 202 degrees Celsius, which is a lot close to the given melting point of the anti-addition product, 202-204 degrees Celsius. The given melting point range was 93.5-95 degrees Celsius. Furthermore, the syn-addition product is unlikely and difficult to produce due to stereochemistry selectivity.
The purpose of this experiment is to perform a two step reductive amination using o-vanillin with p-toluidine to synthesize an imine derivative. In this experiment, 0.386 g of o-vanillin and 0.276 g of p-toluidine were mixed into an Erlenmeyer flask. The o-vanillin turned from a green powder to orange layer as it mixed with p-toludine, which was originally a white solid. Ethanol was added as a solvent for this reaction. Sodium borohydride was added in slow portion as the reducing agent, dissolving the precipitate into a yellowish lime solution.
The possible explanations and changes to make are similar to the previous questions. Conclusion and Future Experiment 18. The identity of the product and unknown were 4-tert-butylbenzyl phenol ether and tert-butyl phenol respectively. The key to making this discovery was the melting point and TLC results!
INTRODUCTION: In this experiment I was testing for antimicrobial sensitivity of Staphylococcus epidermidis by using the Kirby-Bauer Diffusion test. The three antibiotics utilized in this lab were: gentamicin, novobiocin, and penicillin. I determined the effectiveness of the antibiotic by observing and measuring the zone of inhibition for each antibiotic.
Then 1 ml from these bacterial solutions were added to 1 ml of MHII containing different concentration of ciprofloxacin 0.5x, 1x, 5x, 10x, 20x, 30x, 50x,75x and 100x MIC to each well in 12-well plate. Colony counts (CFU/ml) were determined at different time points (T0, T3, T24) by using appropriate dilutions of each culture. Using spot-plating method (32) 10µl was spotted on LB agar plates. However after 24 hour exposure the bacterial cell from dilutions of ≤ 1x102 were washed twice with sterile PBS prior to plating in triplicate. These were then incubated overnight at 37°C.
(Tanta City, Cairo, Egypt). Animals were housed in a room free from any source of chemical contamination, artificially illuminated and thermally controlled at the Animal House Lab., Pharmacology and Chemistry Research Centre, Misr University for Science and Technology (6th October, Giza, Egypt). After an acclimatization period of 1 week, the animals were divided into four groups (10 rats/group) and housed in filter-top polycarbonate cages (five rats per cage). All animals have received human care in compliance with the guidelines of the Animal Care and Use Committee of the Pharmacology and Chemistry Research Centre (6th October City, Giza, Egypt). Infection Model Circular Excision Wound Model For the evaluation of the antibacterial activity, each rat was undergo anaesthesia by intraperitoneal injection of a combination of 10% ketamine hydrochloride (50 mg/kg) and 2% xylazine hydrochloride (5 mg/kg).
Introduction Buffer is a solution that resists a change in pH when bases or acid are added. Solutions that are acidic contain high concentrations of hydrogen ions (H+) and have pH values less than seven. Buffer usually consist of a weak acid, and its conjugate base or a weak base and its conjugate acid. The function of buffer is to resist the changes in hydrogen ion concentration as a result of internal and environmental factor. This buffer experiment is important so that we relies the important of buffer in our life.
Abstract The unknown concentration of benzoic acid used when titrated with standardized 0.1031M NaOH and the solubility was calculated at two different temperatures (20◦C and 30◦C). With the aid of the Van’t Hoff equation, the enthalpy of solution of benzoic acid at those temperatures was determined as 10.82 KJ. This compares well with the value of 10.27KJ found in the literature.
The media used in this experiment was Trypticase nitrate broth. The reagents used (A and B) were sulfanilic acid and alpha-naphthylamine (respectively). Using aseptic technique, the bacterium (16A and 16B) were inoculated into labeled broth test tubes. The tubes were incubated for 48 hours at 37 degrees Celsius. When the incubation was complete 5 drops of reagent A and 5 drops of reagent B were added to each of the broths.