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.
10- Transfer the ester layer to a small dry test tube and dry the ester with anhydrous CaCl2 and stir for 10 min. 11- put it in a preweighed dry round bottom flask . 14- Determine the yield, refractive index, and % yield of ester. Conditions :- 1) This reaction is catalyzed by acid, Like Fischer esterification. 2) Usage of water in step (5):So that after Estrification is completed , any excess unreacted acetic anhydride is hydrolyzed.
Lecturer Date Introduction Theoretical Background Procedure The procedure was segmented into two categories, the reaction set up and the crude product isolation. Reaction set up The magnetic stirrer was prepared through placing it in the fume cupboard. 1 mmol of L-Phenylalanine was placed and weighed in a 5 mL conical vial. After that, a spin vane was inserted into the vial while adding 0.75 mL of 1M H2SO4 solution. During the addition of the sulphuric acid, the solution was stirred at room temperature until the amino acid (L-Phe) completely dissolved.
Then it was left to boil under for 1hour. After which round bottom flask was removed from the reflux setup and held first under running room temperature water and then an ice bath until it cooled down enough to comfortably handle it. Next the cooled solution is poured into a 100ml volumetric flask and topped it off to the mark with denoised water. Subsequently, 20ml of this solution was pipetted into a conical flask. To this, 80ml of cold water and 15ml of 2M HCl was added to the conical flask.
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
Each grounded drug tabled was transferred into a test tube using a spatula. Each test tube was labeled as Tylenol or Anacin. A 2.5ml of 50:50 mixtures of the methylene chloride and ethanol was added to each test tube. The content of each test tube was thoroughly stirred using a glass rod to ensure maximum extraction. The developing chamber for the TLC plates was prepared by adding ethyl acetate that contained 0.5% acetic acid to the glass jar.
Shake c) Drain the lower aqueous layer through the stopcock into the same 250 ml beaker in which the solution had been prepared in steps above. d) Pour the upper solvent layer through the neck of the funnel into a clean 125 ml Erlenmeyer flask. Return the aqueous solution from the 250 ml beaker to the separatory funnel. Add another fresh 20 ml of solvent to the funnel and again extract the aqueous solution as you did in b)
The method was developed on a Novapak C18 (250×4.6mm, 5µ particle size) column using phosphate buffer (pH7.4) and acetonitrile in the ratio of 60:40, v/v as a mobile phase which was pumped at flow rate of 1.0m/min and detection was done at 302nm.the retention time of drug was found to be 7.71min.A prominence isocratic HPLC system (HPLC YL9000 series) with autochro 3000 software an uv detector. A 20 µl hamitton injection syringe was used for sample injection. Preparation of standard and stock solutions 40 mg of Omeprazole was weighed and transferred to 100ml volumetric flask containing 30 ml of 0.1NNaoH. The drug was allowed to dissolved and volume was made up to 100ml with 0.1 Noah. The above solution was diluted with mobile pause to obtain a working standard solution of 40 µg/ml.
Then the bank note was washed by either 20 ml Milli-Q water or 5 ml methanol. The bank note was dried and a second extraction was carried out to calculate the percent recovery. At the primary extraction, different concentration of methanol and PBS were examined. 100 %, 90%, 80%, 70%, 50% methanol: Milli-Q water and PBS were the solvent for extraction. The second extraction was mainly by 100 % methanol.
2. Effects of CMS procedure on sweet food consumption in rats repeatedly treated with amytriptyline or harmine. Bars represent means±S.E.M. * p<0.05). Statistical analysis revealed that CMS rats treated with harmine reverted the reduction of sucrose solution consumption induced by chronic mild stress ([F=3, 27), P=0.012]).