5-aminotetrazole monohydrate: In a 250 ml round-bottom flask equipped with a condenser for refluxing (90 °C) and a magnetic stirring bar, 5.00 g (5.95 mmol) dicyandiamide (three times crystallized), 7.47 g (11.9 mmol) sodium azide and 11.00 g (17.8 mmol) boric acid and 100 ml of water is added and allowed to reflux for 24 hours, after the completion of the reaction, until the solution pH to about 2 to 3 as hydrochloric acid 37% is added (about 12 ml) Then the reaction mixture was cooled in a refrigerator for 18 hours and the white crystals formed. The mixture was filtered and washed three times with 10 ml of water and and dried in 60 °C for 5 hours and finally 45.8 g of product by it will be obtained. 5-Aminotetrazol monohydrate:
2. FORMATION OF HYDRAZONE FROM ESTER Materials required: * The ester which was synthesized in the previous reaction. The total weight of ester obtained was 230mg. * Methanol – 20 ml
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.
Experiment Description: To begin the experiment, 2.0718g of a benzoic acid and p-dichlorobenzene mixture and 30 ml of methylene chloride was placed in a separatory funnel. The funnel was shook to dissolve the contents. After shaking, the funnel was inverted and the stopcock was opened to release the pressure. The stopcock was closed, the funnel was shook, and the pressure was released again. This was repeated until no more gas was released.
2.3. Synthesis of 2-(2-(Morpholinomethyl)-1H-benzimidazol-1-yl)acetohydrazide (4) To a solution of compound 3 (0.01 M, 2.89 g) in methanol (60 mL), 99% hydrazine hydrate (1 mL) was added and the mixture was refluxed for 6 h. The reaction mixture was cooled and the solid thus obtained was filtered, washed with cold water and recrystallized with ethanol to obtain the compound 4. 2.4.
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.
MDA level was determined by thiobarbituric acid reactive substances (TBARS) in serum, based on the reaction between MDA and TBARS. Standard Malondialdehyde solution in 5 mL of volume was processed along with test samples. 1.5 mL of 0.8% of TBA was added to 1 mL of the serum sample. Then 0.4 mL of 8.1% sodium dodecyl sulphate and 1.5 mL of acetic acid was added. 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.
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.
The ion exchange capacity is measured by the chemical titration [Hasimi A, Stavropoulou A, Papadokostaki KG, Sanopoulou M. Euro Polym J (2008) 4098-107]. In order to measure the IEC values, the dry samples were soaked in 1M aqueous NaCl solution at room temperature for 24 hours to exchange of proton by sodium ions. The ion-exchanged NaCl solution was back titrated with 0.1M NaOH solution using phenolphthalein as an indicator. The protonic conductivity measurements were made through via Nyquist plot using N4L PSM 1735 series LCZ meter with amplitude of 10 mV from 1 Hz to 1 MHz The proton conductivity values are calculated
Typically, FeCl2.4H2O (4.3 g) and FeCl3.6H2O (11.6 g) were mixed with 350 mL of deionized water under N2 atmosphere. The resulting solution was heated to 80 °C while stirring, vigorously. Then, 20 mL of 25% NH4OH was quickly added into the solution. The resulting suspension was vigorously stirred for 5 min and then, the black precipitates were collected with the help of a magnet and washed repeatedly with deionized water and ethanol, then dried at vacuum
The silver ion TLC was prepared through the following procedure: Silver nitrate was dissolved in 10 ml of distilled water. This aqueous solution of silver nitrate was absolutely mixed with 9 g of silica gel (10 ~ 40 μm particles). Then, a 10 × 5 cm TLC plate was coated with the above slurry and activated for 1 h at 90 °C before use. They were immediately transferred into a desiccator in dark for storage after cooling. 32 100 μL of afore-prepared sample solution and the mixed reference standard were diluted 100 times with ethyl acetate.
The objective of this experiment was to create synthesize methyl eugenol from eugenol, dimethyl carbonate, and tetrabutylammonium bromide. To start off the experiment, a heating under reflux apparatus was used and the parts included: a water jacketed condenser, ring stand, tubes, flowing water, 25-mL round bottom flask, heating block, and a hot plate. There were two parts to the water condenser, entry and exit ways for water. The bottom opening was connected to the sink through one tube and the top opening was connected with a loose end, which was needed to get rid of the flowing water. To create the solution needed to synthesize methyl eugenol, approximately 0.200 g of eugenol (note: the measured g was converted to mg for later calculations) was measured, alongside approximately 1.2 g of TBAB and was added to the 25-mL round bottom flask.
Experimental Clay-catalyzed dehydration of cyclohexanol Cyclohexanol (10.0336 g, mmol) was added to a 50 mL round bottom flask containing five boiling chips, Montmorillonite K10 clay (1.0430 g) was then added to the cyclohexanol and the mixture was swirled together. The flask was then placed in a sand bath and attached to a simple distillation apparatus. The contents of the flask were then heated at approximately 150 °C to begin refluxing the cyclohexanol. The distillation flask was then loosely covered with aluminum foil and the hood sash was lowered in order to minimize airflow. As the reaction continued, the temperature was adjusted in order to maintain a consistent rate of distillation.
The chemiluminescence part of the experiment, we had to make four solutions labeled as ‘stock solution A, solution A, stock solution B, and solution B’. For the ‘stock solution A’ we put the luminol product, (0.242 g) in a 25 mL Erlenmeyer flask and dissolve it with 2 mL of 3M NaOH. Then we took 1 mL of the ‘stock solution A’ and diluted in 9 mL of water using a 50 mL beaker. Solution A. For the ‘stock solution B’ we mixed 4 mL of potassium ferricyanide solution and 4 mL of hydrogen peroxide solution using a 25 mL Erlenmeyer flask.