4- Set up reflux system using a clean and dry condenser . 5- Place the flask on the hot plate and heat the reaction for 45 minutes - 1 hour . 6- When the reflux is over , remove magnetic stirrer and allow the reaction to cool to room temperature . 7- Add 20 ml of ice water to a separating funnel
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. The solution continued to boil for 25 more minutes until a
The purpose of this experiment was to learn about the electrophilic aromatic substitution reactions that take place on benzene, and how the presence of substituents in the ring affect the orientation of the incoming electrophile. Using acetanilide, as the starting material, glacial acetic acid, sulfuric acid, and nitric acid were mixed and stirred to produce p-nitroacetanilide. In a 125 mL Erlenmeyer flask, 3.305 g of acetanilide were allowed to mix with 5.0 mL of glacial acetic acid. This mixture was warmed in a hot plate with constantly stirring at a lukewarm temperature so as to avoid excess heating. If this happens, the mixture boils and it would be necessary to start the experiment all over again.
1 ml = 1 µg CN (x) Chloramine –T: Dissolve 1 gm chloramine – T in 100 ml distilled water. Prepare fresh solution daily. (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’
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.
In the round-bottom flask (100 mL), we placed p-aminobenzoic acid (1.2 g) and ethanol (12 mL). We swirled the mixture until the solid dissolved completely. We used Pasteur pipet to add concentrated sulfuric acid (1.0 mL) to the flask. We added boiling stone and assembled the reflux. Then, we did reflux for 75 minutes.
Moreover, it acts as dehydrating agent, forcing the equilibrium to the products and lead to a greater yield of ester. After the addition of trace amount of concentrated sulfuric acid, the reactant flask is heated so that the reaction can be speeded up and ester can be obtained faster. The reason of adding concentrated drops-by-drops into the reactant flask and swirl the flask while adding the acid is to prevent any part of the mixture getting too hot and reacting to form unwanted darkly coloured by-product. Before the heating of the liquid, boiling chips is added inside the reactant flask to allow a nucleation site for gradual boiling and avoid a sudden boiling surge where may cause the liquids inside the reactant flask to overflow or spill out as it has
To this, 80ml of cold water and 15ml of 2M HCl was added to the conical flask. Afterwards, 0.1ml of ferroin solution (as an indicator) was added. Next, titration was performed. The contents in the conical flask was titrated with 0.1M ammonia cerium (IV) sulphate until a yellow solution was produced. The experiment was then repeated without sample B (only the H2SO4 and water in the proportion 3:7, 6ml acid 14ml
4- Add HCl acid (acidizing agent) after completing the reaction. 5- layering; concentrating under a lower pressure, add residues into an alcohols solvent for dissolution, add drops of H2O to separate out flucloxacillin crystals 6- Then dissolve Flucloxacillin acid in an organic solvent. 7- Drip Na iso-octoate solution for reaction to produce a product, namely flucloxacillin sodium monohydrate. Step 1: Step 2: Step