Experiment 10: Microwave Chemistry-Synthesis of Phenytoin (Data Sheet) Running the reaction 0.70 g of urea, 1.30 g of benzil, and 0.61 g of sodium hydroxide were ground together in a mortar yielding a yellow power The mixture was transferred to a 25 mL beaker After covering the beaker with a watch glass, it was placed in the microwave and heated for 90 seconds with 280 Watt • The mixture melted and turned pale yellow Product isolation After cooling, the mixture is transferred to a mortar and ground into a powder The solids were extracted twice with 5 mL of 95 % ethanol The combined organic layers were placed in a beaker and 4 mL of 6 M HCl added dropwise; the pH value was below pH=2 and a white precipitate was formed The solids were isolated by vacuum filtration using a Hirsch funnel and rinsed with 2 mL 95 % ethanol The crude was recrystallized from 10 mL of ethanol:water (8:2) The fine needles were isolated by vacuum filtration using a Hirsch funnel and rinsed with 1 mL 95 % ethanol Product characterization 1.65 g of the crude product 1.25 g of the final product • M.p.: 296.5-299.2 °C
Experiment 10: Microwave Chemistry-Synthesis of Phenytoin (Data Sheet) Running the reaction 0.70 g of urea, 1.30 g of benzil, and 0.61 g of sodium hydroxide were ground together in a mortar yielding a yellow power The mixture was transferred to a 25 mL beaker After covering the beaker with a watch glass, it was placed in the microwave and heated for 90 seconds with 280 Watt • The mixture melted and turned pale yellow Product isolation After cooling, the mixture is transferred to a mortar and ground into a powder The solids were extracted twice with 5 mL of 95 % ethanol The combined organic layers were placed in a beaker and 4 mL of 6 M HCl added dropwise; the pH value was below pH=2 and a white precipitate was formed The solids were isolated by vacuum filtration using a Hirsch funnel and rinsed with 2 mL 95 % ethanol The crude was recrystallized from 10 mL of ethanol:water (8:2) The fine needles were isolated by vacuum filtration using a Hirsch funnel and rinsed with 1 mL 95 % ethanol Product characterization 1.65 g of the crude product 1.25 g of the final product • M.p.: 296.5-299.2 °C
Chemistry
10th Edition
ISBN:9781305957404
Author:Steven S. Zumdahl, Susan A. Zumdahl, Donald J. DeCoste
Publisher:Steven S. Zumdahl, Susan A. Zumdahl, Donald J. DeCoste
Chapter1: Chemical Foundations
Section: Chapter Questions
Problem 1RQ: Define and explain the differences between the following terms. a. law and theory b. theory and...
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Please provide experimental percent yield and theoretical yield
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