N-(1-Carboxymethyl-1H-tetrazol-5-yl)-hydrazinium nitrate (3). A solution of AgNO3 (0.10 g, 0.60 mmol) in distilled water (1.5 mL) was added dropwise in the dark to the solution of compound 2 (0.10 g, 0.60 mmol) in Deionized water (1.5 mL) under stirring. After 2-3 hour, the precipitate was filtered, and rinsed with 4 mL distilled water. The solvent was removed by rotary Evaporation to produce a white solid at 88% yield (0.10 g); N-(1-Carboxymethyl-1H-tetrazol-5-yl)-hydrazinium nitrate: Yield: 88%; yellow crystals;. IR (KBr): 3396, 3329, 3140, 3008, 1628, 1494, 1383 cm-1; UV (H2O): λmax = 293-296
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.
Rose Bengal-(bis(aminoethyl)ethylene glycol) (2) from Rose Bengal disodium salt (1) The synthesis was done following procedure from . Rose Bengal Na+ salt (915 mg, 0.90 mmol) was dissolved in DMF (2ml) and DIPEA (0.312 ml, 1.80 mmol), HATU (308 mg, 0.81 mmol) were added. After activation for 15 min, the mixture was added to O-Bis-(aminoethyl)ethylene glycol trityl resin (309 mg, 0.31 mmol) preswollen in DMF for 2 hours. The coupling reaction wrapped in aluminum foil was allowed to proceed overnight on a nitrogen bubbler apparatus. The resulting red-burgundy coloured resin was filtered and washed well with DMF.
How many grams of zinc chloride could be formed from the reaction of 3.57g of zinc with excess HCl? A: 3.75g x 1mol/ 65.39g x 1 mol/ 1mol x 136.4g / 1 mol = 7.45g. 5. Aluminum sulfide reacts with water to form aluminum hydroxide and hydrogen sulfide. (a) Write a balanced equation for this reaction.
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. The mixture was vortexed and after centrifugation at 4000 rpm for 10 minutes, the absorbance of the organic layer (upper layer) was measured in UV-Vis spectrophotometer (Shimatzu) at 532 nm against blank using distilled water. TBA when allowed to react with MDA aerobically formed a colored complex [MDA-(TBA) 2 complex] which was measured with spectrophotometer. MDA concentration (measured as TBARS) was calculated as
2.9. Estimation of Hydrogen peroxide (H2O2) 10 213 The concentration of H2O2 was determined by the method of Okuda et al (38). Fresh leaf 214 sample (0.5 g) was grounded in ice-cold 200 mM HClO4 and was then centrifuged at 215 1200 g for 10 min followed by neutralization of HClO4 of the supernatant with 4M KOH. 216 The insoluble KClO4 was eliminated by further centrifugation at 500g for 3 min. In a 217 total volume of 1.5 mL, the reaction mixture contained 1 mL of the eluate, 400 mL of 218 12.5 mM 3-(dimethylamino) benzoic acid in 0.375 M phosphate buffer (pH 6.5), 80 mL 219 of 3-methyl-2-benzothiazoline hydrazone and 20 mL of peroxidase (0.25 unit).
Isolation of Ibuprofen: Fifteen 200 mg ibuprofen tablets were used, which was 3.37g (16.34 mmol, 112.3%) ibuprofen. This amount of ibuprofen was submerged in 25 mL of acetone and stirred vigorously for 5 minutes to dissolve. Red coatings of the tablet were separated and vacuum filtration was utilized to dissolve all insoluble components. The melting point range of the crude ibuprofen was 72.4-73.9°C. The major bands from the IR are, FTIR: sp3 O-H stretch, about 3200-2500 cm-1 (b, m); sp3 C-H stretch, 2991-2868 cm-1 (sh, m); sp2 =C-H stretch, 3100-3000 cm-1 (sh, w); sp2 C=O stretch, 1701 cm-1 (sh, s); and sp2-sp2, aromatic, C=C stretch (in ring), 1507 cm-1 (s, m).
After the evaluation of stomach for ulcers, the gastric mucosa of glandular portion was scrapped with the help of two glass slides, weighed (100 mg) and homogenized in 1 mL of a 0.15 M, ice cold potassium chloride (KCl) solution and centrifuged at 3,000 RPM for 10 minutes (REMI centrifuge). 1 mL of suspension was taken from the above tissue homogenate in test tube and 0.5 mL of 30% w/v TCA (trichloroacetic acid) was added to it, followed by 0.5 mL of 0.8% w/v TBA (thiobarbituric acid) reagent. The tubes were then covered with aluminium foil and kept in water bath for 30 minutes at 80 °C. After 30 minutes, tubes were taken out and kept in ice-cold water for 30 minutes and centrifuged at 3000 rpm for 15 minutes (R-BC DX REMI centrifuge). The absorbance of the supernatant was read in spectrophotometer (UV-1601, SHIMADZU) at 540 nm against blank.
In this experiment, racemic 2-methylcyclohexanone was reduced using sodium borohydride as a nucleophile to give a diastereomeric mixture of cis and trans secondary alcohols. The products were analyzed for purity using IR spectroscopy and gas chromatography. 1.2 g of 2-methylcyclohexanone and 10 mL of methanol were combined in a flask and cooled in an ice bath. Two 100 mg portions of sodium borohydride were added to the flask and stirred. 5 mL of 3M sodium hydroxide, 5 mL of de-ionized water, and 15 mL of hexane were added to the reaction flask and stirred.
Wash ether layer with saturated sodium chloride solution and retain ether layer. In a small 125ml Erlenmeyer flask, dry the ether solution over anhydrous calcium chloride. Add sufficient calcium chloride so that it no longer clumps to pellets added earlier on the bottom of the flask. Remove the solvent using a rotary evaporator and weigh product. Results 1 mole of benzoic acid (C6H5COOH = 122.12grams) reacts with 1 mole of methanol (CH3OH = 32grams/mole) to produce 1 mole of methyl benzoate (C6H5COOCH3 = 136.15grams) and 1 mole of water.