Aten Ponchung LAB 3-2

Table 1 lists 33 pure compounds, several of which you will select to mix with each of your unknowns, so that you can determine the melting points of the mixtures, and thus the identity of the unknowns.   Table 1.  Known Compounds for Melting Point Experiment     COMPOUND mp range (oC)   COMPOUND mp range (oC)   1)   1,4-dimethoxybenzene   54-56        21)   4-nitroaniline   146-149   2)   2-phenylphenol   57-59        22)   1-napthoic acid   158-160   3)   diphenylacetylene   59-61        23)   salicylic acid   159-161   4)   2,4,6-trichlorophenol   64-66        24)   triphenylmethanol   160-162   5)   biphenyl   68-70        25)   sulfanilamide   165-167   6)   methyl 3-nitrobenzoate   78-80        26)   4-bromoacetanilide   165-169   7)   naphthalene   80-82        27)   itaconic acid   165-168   8)   vanillin   81-83        28)   d-mannitol   166-168   9)…

Given the procedure below to synthesize aspirin, where 30% yield was obtained, what are possible reasons for the lower yield and would this be an effective method to sythesize aspirin on a large scale? Weigh about 2 g of salicylic acid. Record the mass to the nearest milligram. Transfer the solid to a large test tube. Label the test tube. • Carefully add about 4 mL of acetic anhydride to the test tube containing salicylic acid using a 10 mL graduated cylinder. Gently mix the contents, avoiding any spilling of the liquid. Most of the solid will not dissolve at room temperature. • Carefully add about 5 drops of concentrated sulfuric acid to the mixture. Gently swirl to mix the sulfuric acid. • Place your labeled test tube in the hot water bath. After about 1 minute, swirl the contents of the large test tube  to dissolve any salicylic acid that was not dissolved initially. Leave the test tube in the hot water bath for about 15 – 20 min. • While the sample is being heated, fill one-fourth…

If we start with 5.2 g of Benzoic acid, calculate the minimum amount of acid to fully protonate benzoate assuming 90% yield Materials needed for experiment: 7.0 grams of toluene 6.5 mL of 30% sodium hydroxide 60.0 mL of 1M sulfuric acid 19.0 grams potassium permanganate

What are the reagents and chemical groups

4. An unknown compound, Sample 42, is one of the three compounds listed in Table 2: a mixture of Sample 42 with benzoic acid melts at 84-89 °C; a mixture of Sample 42 with phenyl succinate melts at 118-120 °C; and a mixture of Sample 42 with m-aminophenol melts at 101-102 °C. Based on this information, what is the identity of Sample 42? Explain your reasoning. Table 2: Literature melting points for Sample 42 candidates Compound Benzoic acid Phenyl Succinate m-aminophenol mp, °C 121 121 122

4. An unknown compound, Sample 42, is one of the three compounds listed in Table 2: a mixture of Sample 42 with benzoic acid melts at 84-89 °C; a mixture of Sample 42 with phenyl succinate melts at 118-120 °C; and a mixture of Sample 42 with m-aminophenol melts at 101-102 °C. Based on this information, what is the identity of Sample 42? Explain your reasoning. Table 2: Literature melting points for Sample 42 candidates Compound Benzoic acid Phenyl Succinate m-aminophenol 2 mp, ºc 121 121 122

You are employed as a coop student at the Drug and Alcohol Testing Association of Canada (DATAC) developing analytical tests for sports doping agents. You are asked to prepare a procedure for the extraction of methylphenidate, the active compound in Ritalin, from urine samples (consider them as simple aqueous layers, you do not need to consider other components!). The goal of the procedure is to extract the methylphenidate into an organic layer which will then be evaporated, and the residue will be tested for the drug.Your colleague is helping you develop the urine test. They suggest that the urine should be adjusted to a pH above 7 before extracting with the organic solvent. Why is this necessary? Support your explanation with a full arrow-pushing mechanism for the reaction that would occur if the pH was below 7. Include all formal charges, intermediates (if applicable) and products.

You are employed as a coop student at the Drug and Alcohol Testing Association of Canada (DATAC) developing analytical tests for sports doping agents. You are asked to prepare a procedure for the extraction of methylphenidate, the active compound in Ritalin, from urine samples (consider them as simple aqueous layers, you do not need to consider other components!). The goal of the procedure is to extract the methylphenidate into an organic layer which will then be evaporated, and the residue will be tested for the drug.You find that methylphenidate is highly soluble in 2-methyltetrahydrofuran, a bio-renewable solvent. Draw the structure of 2-methyltetrahydrofuran and give two reasons why it is a good solvent choice for liquid-liquid extraction.

1. A compound of molecular formula C5H100 forms a yellow precipitate with reagent and a yellow precipitate with reagents for the iodoform test. 2,4-dinitrophenylhydrazine a) Draw the structural formulae on a piece of paper, take a picture of them and upload the image below. b) Name the two (2) compounds that fit these tests.

Complete the table below with information about the different types of dyes. TYPES OF SUITABLE MEDIUM/ FASTNESS EXAMPLE DYES SUBSTRATE SOLVENT Poor light and wet fast Mauveine Natural Not stated Water Red Lac dye Buff Synthetic Light fast but not wet fast Acid Dye 1) Acid Acid Black 1 Basic Dye 2) 3) Good fastness Basic Red 18 Disperse Blue 165 Disperse Dye Water Good fastness 5) Cellulosic 6) Water Poor fastness polymers Cotton, linen, | 7) Natural dye Indigo Vat and Sulfur Wet fast Dye rayon Wet fast but | 9) poor light fast 8) Cotton, nylon Water Cellulosic 10) Reactive Blue Reactive Dye Water fibers 19

Answer the following questions. What are the reasons for determining the ash content of a drug? What is the purpose of heating the crucible to dull redness until a constant weight is obtained? What are the possible contents of the Total Ash and Acid-Insoluble Ash obtained from the sample drug used?

Data: Density of p-phenetidine is 1.065g/mol Williamson Ether Synthesis: Mass of filter paper:   0.680 g Mass of filter paper and product:  1.482 g Melting Point:  134-136oC Amide Synthesis: Mass of filter paper:   0.686 g Mass of filter paper and product: 1.589 g Melting Point:  135-137oC Mixed Melting Point (product of amide synthesis mixed with Williamson Ether synthesis product): 134-136oC (a)Calculate theoretical yield of both williamson ether synthesis of phenacetine and amide synthesis of phenacetin. (b) calculate the percent yield of phenacetin obtained via williamson ether synthesis. (c) Calculate the percent yeild of phenacetin obtained via the amide synthesis.

how would one devise in carry out an experiment to determine which one of these compounds is the unknown?

In greater details, describe the differences you would see when conducting the nitrous acid test on aniline vs. propyl amine. Be specific.

Which question will your experiment investigate? (select one and delete the others) How does temperature affect how lactase drops work to break down lactose into glucose and galactose? How does pH affect how lactase drops work to break down lactose into glucose and galactose? How does agitation (movement) affect how lactase drops work to break down lactose into glucose and galactose? What variable will you change in this experiment? This is also called the Independent variable. How will you change it? What variable will you measure in this experiment to determine the effect of the variable you changed? This is also called the Dependent variable. How will you measure it? What variables will you keep the same in this experiment? Check off the items in this list that you would use for this experiment. You may add any items you feel you would need. O skim milk (which contains lactose) O Lactase drops O Graduated cylinder Eye dropper Ice cubes O pH paper O Hot plate Mixing spoon O…

In diluting acid solution, which of the following statements are correct? I. Add the acid into distilled water to dilute the acid solution II. Add distilled water into acid to dilute the acid solution III. Use serological pipette in transferring acid into a beaker containing distilled water IV. Use serological pipette in transferring distilled water into a beaker containing acid O I and IV O Il and IV Il and III T and II

Ans

methyl alcohol and ethyl alcohol are poor extraction solvent. why?

Part B: Miscibility of liquids 1. Place 10 drops of propan-2-ol into each of two DRY semi-micro test tubes. 2. Add 10 drops of water to one test tube and 10 drops of cyclohexane to the other test tube, shake and observe whether the two liquids in each test tube are miscible. Record your results then discard the contents of the test tubes into the organic waste container. 3. Place 10 drops of water in a clean semi–micro test tube and add 10 drops of cyclohexane to it. Record whether the two liquids are miscible. If two layers form (i.e. the liquids are immiscible) add a drop of blue food dye to the mixture and shake, then allow the two layers to reform. Based on your observation, decide whether the food dye is more soluble in water or cyclohexane and then discard the mixture into the non–halogenated waste container. Record whether the combinations of liquids shown below are miscible. Water Cyclohexane Propan-2-ol Cyclohexane

An old sample of cinnamaldehyde analyzed by TLC and visualized with a UV lamp. Explain why the contaminant, cinnamic acid, appears below the cinnamaldehyde spot.