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.
2. Mix a combination of the NaClO and the thiosulfate solution equal to 50 ml in a Styrofoam cup, stir with thermometer, and record temperature in the data table. Dispose of solutions and rinse cup well. Continue taking data until you have enough data to record and make a thorough graph. 3.
Cross Condensation of aldol 2015007632 Dowrie, K Contents Reaction 1 Introduction 1 Experiment Procedure 2 Experimental results 3 Table of calculations 3 Calculations 3 NMR 4 TLC 4 References 5 Reaction Introduction An aldehyde reaction is when aldehydes and keytones, both containing an α-hydrogen in the presence of an alkali group condenses and forms an enone. Acetone has α-hydrogens on each side. The proton can be removed and therefore giving a nucleophile anion. The aldehyde carbonyl is more reactive than the keytone and so it reacts rapidly with the anion. This product undergoes base catalysed hydration giving dibenzalacetone.
Degradation study of Product 01 using Aqueous 1N NaOH solution .The mechanism is operated by hydrolysis. The hydroxyl group (-OH) of NaOH attacks an electrophilic carbon of >C=O group which an removal of tertiary Nitrogen gives 4-MBA and PD as by products. Degradation study of Product 02 using Aqueous 1N NaOH solution . The mechanism is operated by hydrolysis. The hydroxyl group (-OH) of NaOH attacks an electrophilic carbon of >N-C=O which as rearrangement gives carbonial .
8. Record the temperature every 30 seconds for a total of 10 minutes. ￼￼￼Chemicals ￼￼￼￼￼￼￼Quantity ￼￼￼￼Sodium chloride powder (NaCl(s)) ￼￼20 g ￼￼￼Water ￼￼￼￼￼￼￼500 ml ￼￼￼Page 5 of 7 9. Repeat steps 4 to 8 for a total of 3 recordings. Making sure that all the apparatus are washed thoroughly before each experiment.
In this lab, the oxidation of a secondary alcohol was performed and analyzed. An environmentally friendly reagent, sodium hypochlorite, was used to oxidize the alcohol, and an IR spectrum was obtained in order to identify the starting compound and final product. The starting compound could have been one of four alcohols, cyclopentanol, cyclohexanol, 3-heptanol, or 2-heptanol. Since these were the only four initial compounds, the ketone obtained at the end of the experiment could only be one of four products, cyclopentanone, cyclohexanone, 3-heptanone, or 2-heptanone. In order to retrieve one of these ketones, first 1.75g of unknown D was obtained.
There is one mole of OH- in the solution since NaOH goes to Na+ and OH-. Trial 1: 25.65mL NaOH x 0.100mol/1000mL = 2.57 x 10-3 mol NaOH = 2.57 x 10-3 mol HA = 2.57 x 10-3 mol H+. The equivalent mass is 0.356g Acid / 2.57 x 10-3 mol H+ = 139g/mol H+ Trial 2: 49.57mL NaOH x 0.100 mol / 1000 mL = 4.96 x 10-3 mol NaOH = 4.96 x 10-3 mol HA = 4.96 x 10-3 mol H+. The equivalent mass is 0.644g Acid / 4.96 x 10-3 mol H+ = 130.g/mol H+ Average = (139g Acid / 1 mol H+) + (130.g Acid / 1 mol H+) / 2 = 135g/mol H+. The average equivalent mass for the acid is 135g/mol H+.
The drop rate was adjusted to 1 to 2 drops/second. 10.0 mL of the NaOH solution was allowed to drip away into a waste beaker. The exact volume of the sodium hydroxide solution used was determined. A clean 250-mL beaker was taken and around 0.3 to 0.5 g of potassium acid phthalate was weighed into it. 50 mL of distilled water was approximately added to this 250 mL beaker and gently swirled so that the solid (potassium acid phthalate) got fully dissolved into the water.