Chloroacetic acid (0.5 g, 5. 28 mmol), 5-aminotetrazole monohydrate (0.45 g, 5. 28 mmol), and sodium hydroxide (0.59 g, 10.57 mmol) in 10 ml of water was refluxed 20 hr, cooled, and made strongly acidic with concentrated hydrochloric acid. The mixture was cooled overnight and precipitate was separated to give 0.28 g a white solid product at 45.41% yield. (5-Amino-tetrazol-1-yl)-acetic acid: Yield: 45.41%; white crystals; m.p 210-213°C; IR (KBr): 3388, 3315, 3270, 3205, 3010, 2976, 1697, 1638, 1586, 1496, 1257 cm-1; 13C NMR (75 MHz (DMSO-d6)): 168, 156,
Then, Fe(NO3)3·9H2O (0.5mol) was added to above solution and was kept at 80 °C for 12h under reflux. The obtained red-brown solid was filtered and washed for three times with methanol and DMF, then dried in air. The as-prepared photocatalyst was characterized by SEM (VP-1450), EDX (type
* In the above RB, a calculated amount of 1.2 equivalent amount of PTSH was added during continous stirring. * To the RB a condenser was attached and it was put on refluxing for a time period of 18 hours at a temperature of 80 degrees in an oil bath. * Post refluxing, the condenser was removed and it was left undisturbed for 1 day and then cooled to a temperature of -20 degrees by keeping in the freezer for setting of hydrazone crystals. * Once the crystals were formed, the supernatant was decanted and the crystals were transferred to a beaker where they were washed with cold methanol and then dried. * These dried hydrazone crystals were used in the subsequent steps.
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.
Heat the solution until it is at 100 ˚C then continue heating for 75 minutes. Evolution of CO2 and NH3 is observed during heating. e. After 75 minutes of heating, stop stirring. Draw a little clear solution with a pipette, cool the solution to room temperature and measure its pH value with pH paper. when the pH is 7, allow the solution to cool to room temperature.
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. The mixture was transferred to a separatory funnel, separated into an organic layer and water layer, and then drained. The water layer was washed twice with 10 mL of hexane. The organic layer was dried
2.4.1. Tetramethyl glucose acetylation 1gm of tetramethyl glucose was dissolved in 5ml of acetic anhydride and added to fused sodium acetate of 0.375gm and mixed for 10 minutes and allowed to cool. To this mixture 7.5ml of toluene and 5ml of dry ether were added. The whole mixture evaporated to syrup on a water bath at 50 °C. The product dissolved in the dry ether after washing with toluene.
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
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).
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
Methanol was filled in a test tube and placed into a water bath to heat up. 12 Drops of the Methanol were then added to each flask until the crude caffeine had completely dissolved. 13. The solution was then filtered and the residue collected in a filter paper. It was left to dry and
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.