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Start the reaction and use magnetic stirring. Monitor the reaction by TLC at 30, 60 and 90 minutes comparing with authentic standards.
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Mark all spots that you see, tracing their outlines with a pencil and calculate the retention factor RF. After completion of the reaction, evaporate the solvent of the round-bottom flask in a rotavapor.
Remove the solution with a Pasteur pipette and pour it into a test tube.
Add 3 mL of water and shake vigorously. Evaporate the solvent in a rotavapor and observe the formation of a silky white solid 0. By determining the melting point and comparing it with the authentic standard m.
Reaction by heating Prepare a reflux set-up and pre-heat a sand bath. In a 5 mL round-bottom flask equipped with a magnetic barsuspend 0.
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After this time the reaction will be monitored by TLC comparing with authentic standards. Then add 1 mL of CH2Cl2 and stir manually until the product dissolves. Add 4 mL of CH2Cl2 over sodium sulphate for washing, always recovering the liquid in the round-bottom flask.
Hazards Ultraviolet light is damaging to the skin and eyes. The UV lamps used for visualization of the analytes on fluorescent TLC plates should always face downward, and students should take care not to look directly into them.
Methyl iodide is a volatile liquid and exhibits moderate to high acute toxicity by inhalation, and skin contact may cause irritation and dermatitis.
Both methanol and sodium methoxide are toxic. Methanol is toxic both by ingestion and inhalation, and therefore reactions with this solvent should be carried out in a fume hood. Sodium methoxide causes topical burns because it is hydrolyzed on the skin to sodium hydroxide.
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