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,
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.
Using filtration sodium acetate was separated, and the filtrate was evaporated to obtain syrup and fractionated at a boiling point of 133-136 °C. The obtained product dissolved in hydrogen bromide of glacial acetic acid and this mixture reaction kept in an ice bath for 1hr. According to procedure, the product was methylated to obtain 1bromo-2, 3, 4, 6-tetramethylglucose.
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.
The washings are filtered off into a 100 mL measuring flask; after cooling distilled water is added until the mark is reached (stock solution). In proportion to the expected chloride content aliquot part of this solution, which should preferably contain 50 mg – 100 mg NaCl, taken off, distilled water being added to obtain a quantity of approximately 100 mL. Subsequently 5 mL ferric alum solution, 20 mL 0.1 N AgNO3 solution and 5 mL – 10 mL ether or 1 mL nitrobenzene are added; titration is carried out by means of an ammonium thiocyanate solution 0.1 N, until the red colouring remains after
A spin vane was added and a water-jacked condenser was attached. Isopentyl nitrite (0.06ml, 0.045 mmol) was dissolved in 1,2-dimethoxyethane (0.50 ml) in a 3-ml conical vial and caped to prevent loss by evaporation. Running the reaction. The mixture in the 5-ml conical vial containing the tetraphenylcyclopentadienone and anthranilic acid was heated on an aluminum block to 140° C. Once the mixture started to boil the prepared mixture of isopentyl nitrite was added to the 5-ml conical vial through the top of the condenser using a pasture pipette.
Throughout the mixing process, the clear red solution slowly changes to a denser red solution (Appendix figure 23). A thermometer was used for temperature checking. The beaker was removed from the hot plate when the temperature was found to be higher than 50 ℃. This was done to prevent a sudden gelation happen before all the active dissolved in the ethylene glycol. Moderate heating of the solution for a period of time is allowed to obtain a wet gel (Appendix figure 24).
Shake funnel and rinse off water layer ( This contains the sulfuric acid and majority of methanol). Again wash the ether with 25ml of water and then wash the organic layer with 25ml of 10% sodium bicarbonate to extract unreacted benzoic acid. Again shake separatory funnel with frequent venting of pressure and opening the stopcock. Allow the separation of layers and drain off bicarbonate layer into a beaker. Wash ether layer with saturated sodium chloride solution and retain ether layer.
Procedure a. Weigh 40 g urea and 3.15 g of oxalic acid, put them into a 250 ml Erlenmeyer flask. Add 18 mL water. Heat them at 70 ˚C until the mixture totally dissolve. c. weigh 1.900 g Ba(NO3)2, 2.635 g Cu(NO3)2‧3H2O and 1.393 g Y(NO3)3‧6H2O
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.
5. 150 ml of the solution in beaker A was added to the separating funnel with 10ml of chloroform. The funnel was gently shaken and vented to release the pressure. This was done five times. 6.
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.