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Lab at Mahidol

Date post: 27-Jun-2015
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Nitchanan Kwanlertchit Bhuree Dardarananda
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Synthesis Dicyclopentadienone
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Page 1: Lab at Mahidol

SynthesisDicyclopentadienone

Page 2: Lab at Mahidol

NANOTECHNOLOGY REVOLUTION

Page 3: Lab at Mahidol
Page 4: Lab at Mahidol

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.

Page 5: Lab at Mahidol
Page 6: Lab at Mahidol

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.

Page 7: Lab at Mahidol

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

Page 8: Lab at Mahidol

-OBJECTIVES

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

Page 9: Lab at Mahidol

-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)

Page 10: Lab at Mahidol

-CHEMICAL

• Fe-B(OH)3

•K2CO3

•Na2SO4

•H2SO4

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

Page 11: Lab at Mahidol

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

Page 12: Lab at Mahidol

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

Page 13: Lab at Mahidol

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

Page 14: Lab at Mahidol

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

Page 15: Lab at Mahidol

Result & discussion

Spectrum of dicyclopentadienone

Fe-B(OH)3 dicyclopentadienone

2-Aminothiophenol KOH

Page 16: Lab at Mahidol

Spectrum of dicyclopentadienone

Fe-B(OH)3 dicyclopentadienone

K2CO3

Au

Page 17: Lab at Mahidol

Spectrum of dicyclopentadienone

Fe-B(OH)3 dicyclopentadienone

KCO3 Au sponge

Page 18: Lab at Mahidol

Spectrum of dicyclopentadienone

Fe-B(OH)3 dicyclopentadienone

KCO3 Au nano

Page 19: Lab at Mahidol

Analysis

Page 20: Lab at Mahidol

Work up

Page 21: Lab at Mahidol

Done by :Nitchanan

Kwanlertchit(Mint)

Bhuree Dardarananda(

Pooh)

Page 22: Lab at Mahidol

Thank you Dr.Ekasith Somsook

and P’Pikky


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