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
Transcribed Image Text: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
М.р.: 296.5-299.2 °C
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