Lab Report- Exp 1 Diels Alder Reaction

Lab Report Exp 1 Diels Alder Reaction

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Unformatted text preview: recrystallization. After allowing the vial to recrystallize on ice for 10 minutes, a glass stirring rod was used to scratch the inside of the conical vial and a white slush liquid appeared while crystals formed. The solution containing the crystals was then put through the vacuum filter. The vial and crystals were rinsed with 1 mL of cold petroleum ether. White crystals resulted with a brown tint due to the heating of the boiling stones. The crystals were then emptied into a pre-weighed aluminum tray. The tray weighed 1.369 grams without the crystals and 1.416 grams with the crystals. The mass of the crystals was 0.047 grams when weighed the first time and a week later they were reweighed and totaled 0.046 grams. The solid crystalline product is cyclohex-4-ene-1,2dicarboxylic anhydride and the melting point was also measured and determined to be 92.794.2oC. The limiting reagent was determined to be maleic anhydride at 9.68x10-4 mols, this was then multiplied by 152.15 g/mol, the molecular weight of cyclohex-4-ene-1,2-dicarboxylic anhydride, to give the theoretical yield of 0.147 grams cyclohex-4-ene-1,2-dicarboxylic anhydride. The mass of the dried crystals, 0.046 g was then divided by the theoretical yield of 0.147 g and multiplied by 100 to give the percent yield of the product which was approximately 31.3%. All physical data can be seen in Data Table 2 and calculations are below. Figure 3: Reflux Apparatus4 Calculations and Data: Maleic Anhydride: (0.095 g) / (98.06 g/mol) = 9.68 x 10-4 mol = limiting reagent Butadiene: (0.207 g) / (118.11 g/mol) = 1.75 x 10-3 mol Theoretical Yield: 9.68 x 10-4 mol x 152.15 g/mol C8H8O3 = 0.147 g Cyclohex-4-ene-1,2dicarboxylic Anhydride Percent Yield: (0.046 g obtained product) / (0.147 g) x 100 = 31.3% Data Table 2: Compound Mass Crystals Week 1 Cyclohex-4-ene-1,2dicarboxylic Anhydride 0.047 g Mass Crystals Week 2 0.046 g Melting Point 1 92.7-94.2 oC Melting Point 2 93.2-94.3 oC Literature Melting Point Percent Yield 103-104 oC 3...
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This document was uploaded on 04/06/2014.

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