Pour the hot reaction mixture now out into a petridish, covered with a paper to prevent loss by sublimation, and allow to cool. Step II: Preparation of anthranilic acid from pthalimide Reaction: (Step 2 is Hoffmann degradation reaction) Procedure: 4. Dissolve 15 g sodium hydroxide in 15 ml water. Keep the solution cool and add 4.2 mL bromine in one lot. 5.
The absorbance of the supernatant was read at 540 nm at room temperature against appropriate blank. Blank consist of 1 ml distilled water, 0.5 ml of 30% TCA, and 0.5 ml of 0.8% TBA. TBARS values were expressed as n moles malonaldehyde (MDA)/mg protein. Estimation of
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.
The sample was transferred to a 250 ml conical flask kept in water bath for alkali treatment. 75 ml of 17.5% caustic soda was measured using a measuring cylinder at 20°C. 15 ml of 17.5% NaOH was added and fibres were macerated gently with a flattened glass rod for 1 minute. 10 ml more NaOH was added and the solution was mixed for 45 seconds. 10 ml NaOH was again added and mixed for 15 seconds to make lump free slurry.
Bromination is a type of electrophilic aromatic substitution reaction where one hydrogen atom of benzene or benzene derivative is replaced by bromine due to an electrophilic attack on the benzene ring. The purpose of this experiment is to undergo bromination reaction of acetanilide and aniline to form 4-bromoacetanilide and 2,4,6-tribromoaniline respectively. Since -NHCOCH3 of acetanilide and -NH2 of aniline are electron donating groups, they are ortho/para directors due to resonance stabilized structure. Even though the electron donating groups activate the benzene ring, their reactivities are different and result in the formation of different products during bromination.
(xi) Pyridine (xii) 1-phenyl–3-methyl– 5-pyrazolone solution: Prepare a saturated aqueous solution (approximately 0.5 gm / 100 ml) by adding the pyrazolone to water at 75 0 C. Agitate occasionally as the solution cools to room temperature. (xiii) Bis–Pyrazolone (3,3-dimethyl-1-diphenyl) (4,4’-bis-2-pyrazolone)-(5,5’
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. The mixture was vigorously shaken and left to stand at room temperature for 10 min. Absorbance was measured at 562 nm after 10 min.8 % Inhibition = [(AB - AA)/AB] x 100, where AB, absorption of blank sample, AA, absorption of test sample.
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:
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.
Figure 2.2 shows that the reaction of ethane-1,2-diol with benzene-1,4-dicarboxylic
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
The objective of this experiment was to use an aldol condensation reaction to synthesize 3-nitrochalcone from 3- nitrobenzaldehyde. This was accomplished with a Diels-Alder reaction that utilized 3-nitrobenzaldehyde, acetophenone, ethanol, and sodium hydroxide. The mechanism for the synthesis of 3-nitrochalcone is presented in Figures 1 and 2. The alpha carbon on the acetophenone is deprotonated. This is followed by the attack of the alpha carbon anion on the carbonyl carbon on the 3-nitrobenzaldehyde.