Lab at Mahidol

Post on 27-Jun-2015

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Nitchanan Kwanlertchit Bhuree Dardarananda

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SynthesisDicyclopentadienone

NANOTECHNOLOGY REVOLUTION

The use of nanotechnology

Nanotechnology, basically, deals with controlling and modifying matter at molecular and atomic scale. The physical properties of matter change dramatically as its surface to area ratio is increased to nano scales. For instance, the elements that are known to be inert start functioning as catalyst. Similarly, materials develop unique colloidal properties, solubility capacity and electrical properties. Such materials find a wide variety of application in fields as diverse as electronics, medicine and energy production.

CATALYSIS

Catalysis is the process by which the rate of a chemical reaction is increased by means of the addition of a species known as a catalyst to the reaction.

There are two type of catalyst, the heterozygous and the homozygous in this experiment, the catalyst that we chose to use is a heterozygous. Which is a insoluble and a easy to separated catalyst.

TYPE OF CATALYST

Homogeneous • Insoluble

• Hard to separated

• Use low T and P

• High selectivity

• Easy to modify

Heterogeneous • Insoluble

• Easy to separated

• Use high T and P

• Poor selectivity

• Difficult to modify

-OBJECTIVES

• Want to synthesize dicyclopentadienone.• Study the results of the catalyst, to see if a reactions occur or not.• Purify by using chromatography.

-MATERIALS LIST

• Glass• Flasks• Dropper•Cylinder•Beaker• Column• Watch glass• Pipette• Transfer pipette• NMR tube• Petri dish • Spectular

(INSTRUMENT)

• Magnetic stirrer• magnetic bar• Nuclear magnetic resonance spectroscopy (NMR)• Cooling ace• Rotavapour• UV lamp• Acetone• Vial• Glove• Paraflim• Foil• Forseps• Thin layer chromatography

(GLASS)

-CHEMICAL

• Fe-B(OH)3

•K2CO3

•Na2SO4

•H2SO4

•EtoAc•Hexane•Au sponge•Au nano•THF•Chloroform•Deionized water

Fe-B(OH)3 dicyclopentadienone

•Fe-B(OH)3 0.0575 g•KOH

0.0421 g•2-aminothiophenol 54 μlit•H2O 15 ml•EtoAc•Hexane

Procedure:1.weight the ferroceneboronic acid (0.0575g) the substrate of KOH is 0.0421g weight the 2-aminothiophenol substrate 54 ml2. put the ferroceneboronic acid into a beaker then follow by the KOH into the same beaker.3.add 15ml of H2O into the same beaker.4.Use magnetic bar to stir with 80°C5. take the chemical out6. put the solution in a separation funnel.7. separate until the solution is pure8. After ,use the chromatography with the solution, substrate and product.9. check the results with NMR

Conclusion: the result shows that nothing happen in this experiment

Fe-B(OH)3 dicyclopentadienone

Fe-B(OH)3 0.2 gK2CO3 0.36 gTHF 4 mlH2O 6 mlAu 0.144gEtoAc Hexane

Procedure:1.weight the ferroceneboronic acid 0.2g, the substrate of K2CO3 is 0.36g weight the Au substrate 0.144 g 2. put the ferroceneboronic acid into a beaker then follow by the K2CO3 into the same beaker.3.add 6ml of H2O into the same beaker.4.Use magnetic bar to stir with room temp for 24 hours 5. take the chemical out6. put the solution in a separation funnel.7. separate until the solution is pure8. After ,use the chromatography with the solution then test substrate and product by TLC test. 9. check the results with NMR

Conclusion: the result shows that nothing happen in this experiment

K2CO3

Au

Fe-B(OH)3 dicyclopentadienone

Fe-B(OH)3 0.2 gK2CO3 0.36 gTHF 4 mlH2O 6 mlAu sponge 0.144gEtoAc Hexane

Procedure:1.weight the ferroceneboronic acid 0.2g, the substrate of K2CO3 is 0.36g weight the Au sponge substrate 0.144 g 2. put the ferroceneboronic acid into a beaker then follow by the K2CO3 into the same beaker.3.add 6ml of H2O into the same beaker.4.Use magnetic bar to stir with room temp for 24 hours 5. take the chemical out6. put the solution in a separation funnel.7. separate until the solution is pure8. After ,use the chromatography with the solution then test substrate and product by TLC test. 9. check the results with NMR

Conclusion: the result shows that nothing happen in this experiment

KCO3 Au sponge

Fe-B(OH)3 dicyclopentadienone

Fe-B(OH)3 0.2 gK2CO3 0.36 gTHF 4 mlH2O 6 mlAu nano 20 mgEtoAc Hexane

Procedure:1.weight the ferroceneboronic acid 0.2g, the substrate of K2CO3 is 0.36g weight the Au nano substrate 20 mg2. put the ferroceneboronic acid into a beaker then follow by the K2CO3 into the same beaker.3.add 6ml of H2O into the same beaker.4.Use magnetic bar to stir with room temp for 24 hours 5. take the chemical out6. put the solution in a separation funnel.7. separate until the solution is pure8. After ,use the chromatography with the solution then test substrate and product by TLC test. 9. check the results with NMRConclusion: the result shows that nothing happen in this

experiment

KCO3 Au nano

Result & discussion

Spectrum of dicyclopentadienone

Fe-B(OH)3 dicyclopentadienone

2-Aminothiophenol KOH

Spectrum of dicyclopentadienone

Fe-B(OH)3 dicyclopentadienone

K2CO3

Au

Spectrum of dicyclopentadienone

Fe-B(OH)3 dicyclopentadienone

KCO3 Au sponge

Spectrum of dicyclopentadienone

Fe-B(OH)3 dicyclopentadienone

KCO3 Au nano

Analysis

Work up

Done by :Nitchanan

Kwanlertchit(Mint)

Bhuree Dardarananda(

Pooh)

Thank you Dr.Ekasith Somsook

and P’Pikky