Promieniowanie mikrofalowe w ... - Dydaktyka...
Transcript of Promieniowanie mikrofalowe w ... - Dydaktyka...
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Promieniowanie mikrofalowe w chemii organicznej
Alicja Kluczyk
18 stycznia 2016
Kuchenka mikrofalowa
naczynia
potrawy
czas
moc
ilo materiau
czego nie naley wkada do mikrofalwki?
https://www.youtube.com/watch?v=t0Gw50o7iuA
https://www.youtube.com/watch?v=9F1KUp4G1uo
Rys historyczny
nieprzewidziane konsekwencje zastosowania
radaru czyli co Percy LeBaron Spencer nosi
w kieszeni
baton orzechowy
popcorn
jajko
Percy LeBaron Spencer
http://www.gallawa.com/microtech/history.html
Kuchenny rys historyczny
1947 RADARANGE (2 000-3 000 $)
1952-55 model domowy (1 295 $) 2450 MHz
Panasonic NE1846 6 999 z
AEG Micromat Combi 3880 E-M 3 300 z 140 z
https://www.youtube.com/watch?v=t0Gw50o7iuAhttps://www.youtube.com/watch?v=t0Gw50o7iuAhttps://www.youtube.com/watch?v=t0Gw50o7iuAhttp://en.wikipedia.org/wiki/File:Magnetron_section_transverse_to_axis.JPG
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B. L. Hayes, Microwave synthesis, CEM Publishing, 2002
Parametry
staa dielektryczna '
strata dielektryczna
przeksztacanie energii mikrofal w ciepo
tan (tan = / )
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Jak uzyska wysok temperatur dla niskowrzcego rozpuszczalnika?
Zastosowania naukowe
microwave synthesis
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2013: 2 518 prac w Web of Science
2014: 2 614
2015: 2 538
Mineralizatory i ekstraktory Syntezator mikrofalowy CEM Discover
http://cem.com/page153.htmlhttp://cem.com/page36.htmlhttp://cem.com/page37.htmlhttp://cem.com/page38.htmlhttp://cem.com/page39.html
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http://www.anton-paar.com/001/en/60/557 http://www.anton-paar.com/001/en/60/557
Microwave SPPS System
Mikrofale i .
fotochemia
synteza organiczna (warunki homogeniczne)
synteza organiczna na noniku staym * **
chemia zwizkw heterocyklicznych
katalizatory metale przejciowe
cykloaddycja
odczynnki na noniku
reaktory cinieniowe
radiochemia
kataliza homogeniczna
efekty nietermiczne *
katalizatory przeniesienia fazowego
Reakcje wspomagane
MAOS
Microwave-Assisted Organic Synthesis
MEC
Microwave-Enhanced Chemistry
MORE
Microwave-organic Reaction Enhancement
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Proste przykady
Green chemistry
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Title: Microwave-assisted stereoselective alpha-2-deoxyglycosylation of hex-1-en-3-uloses Author(s): Lin HC, Wu HH, Lin ZP, et al. Source: TETRAHEDRON LETTERS Volume: 50 Issue: 52 Pages: 7327-7329 Published: DEC 30 2009
Title: Microwave-assisted McMurry polymerization utilizing low-valent titanium for the synthesis of poly 2,6-[1,5-bis(dodecyloxy)naphthylene vinylene] (PNV) Author(s): Thomas H, Stuhr-Hansen N, Westerlund F, et al. Source: TETRAHEDRON LETTERS Volume: 50 Issue: 52 Pages: 7374-7378 Published: DEC 30 2009
Title: Microwave-Assisted, Rapid, Solvent-Free Aza-Michael Reaction by Perchloric Acid Impregnated on Silica Gel Author(s): Singh SP, Kumar TV, Chandrasekharam M, et al. Source: SYNTHETIC COMMUNICATIONS Volume: 39 Issue: 22 Pages: 3982-3989 Published: 2009
Title: Novel One-Pot Synthesis of 3-Phenylnaphtho[2,3-b]furan and 3-Phenylbenzofurans Under Microwave Irradiation and Solvent-Free Conditions Author(s): Wang ZX, Gu JZ, Jing HW, et al. Source: SYNTHETIC COMMUNICATIONS Volume: 39 Issue: 22 Pages: 4079-4087 Published: 2009
Title: Synthesis and characterization of Eu-doped hydroxyapatite through a microwave assisted microemulsion process Author(s): Yang C, Yang PP, Wang WX, et al. Source: SOLID STATE SCIENCES Volume: 11 Issue: 11 Pages: 1923-1928 Published: NOV 2009
Title: Synthesis, Spectral and Biological Evaluation of Some Mesoporphyrinic Zn(II) Complexes Author(s): Boscencu R, Socoteanu R, Ilie M, et al. Source: REVISTA DE CHIMIE Volume: 60 Issue: 10 Pages: 1006-1011 Published: OCT 2009
Title: Synthesis and Antimicrobial Activity of New Aromatic Esters of Potential Interest in Supramolecular Chemistry Author(s): Balan AM, Zbancioc G, Bentea E, et al. Source: REVISTA DE CHIMIE Volume: 60 Issue: 10 Pages: 1021-1024 Published: OCT 2009
Title: Synthesis of Novel Flower-Like Zn(OH)F via a Microwave-Assisted Ionic Liquid Route and Transformation into Nanoporous ZnO by Heat Treatment Author(s): Song JK, Zheng MB, Yang ZJ, et al. Source: NANOSCALE RESEARCH LETTERS Volume: 4 Issue: 12 Pages: 1512-1516 Published: DEC 2009
Title: Microwave-assisted solid-phase peptide synthesis at 60 degrees C: alternative conditions with low enantiomerization Author(s): Loffredo C, Assuncao NA, Gerhardt J, et al. Source: JOURNAL OF PEPTIDE SCIENCE Volume: 15 Issue: 12 Pages: 808-817 Published: DEC 2009
Title: Microwave-assisted synthesis of ZnO micro-javelins Author(s): Padmanabhan SC, Ledwith D, Pillai SC, et al. Source: JOURNAL OF MATERIALS CHEMISTRY Volume: 19 Issue: 48 Pages: 9250-9259 Published: 2009
brak
rozpuszczalnika
selektywno
ciecze jonowe
nonik stay **
nonik stay *
1.
Microwave-Assisted Bleaching of Wool Fabrics
By: Abou El-Kheir, Amira; Haggag, Karima; Mowafi, Salwa I.; et al.
JOURNAL OF NATURAL FIBERS Volume: 12 Issue: 2 Pages: 97-107 Published: MAR 4 2015
2.
Microwave-assisted synthesis of graphene-Ni composites with enhanced microwave absorption properties in Ku-band
By: Zhu, Zetao; Sun, Xin; Li, Guoxian; et al.
JOURNAL OF MAGNETISM AND MAGNETIC MATERIALS Volume: 377 Pages: 95-103 Published: MAR 1 2015
3.
Single-crystalline AgIn(MoO4)(2) nanosheets grafted Ag/AgBr composites with enhanced plasmonic photocatalytic activity for
degradation of tetracycline under visible light
By: Yan, Xu; Wang, Xiyou; Gu, Wei; et al.
APPLIED CATALYSIS B-ENVIRONMENTAL Volume: 164 Pages: 297-304 Published: MAR 2015
4.
Inhibition of photocorrosion and photoactivity enhancement for ZnO via specific hollow ZnO core/ZnS shell structure
By: Yu, Linhui; Chen, Wei; Li, Danzhen; et al.
APPLIED CATALYSIS B-ENVIRONMENTAL Volume: 164 Pages: 453-461 Published: MAR 2015
5.
Preparation, characterisation and physicochemical properties of the phosphate modified peanut protein obtained from
Arachin Conarachin L.
By: Yu, Lina; Yang, Weiqiang; Sun, Jie; et al.
FOOD CHEMISTRY Volume: 170 Pages: 169-179 Published: MAR 1 2015
6.
Optimisation and validation of the microwave-assisted extraction of phenolic compounds from rice grains
By: Setyaningsih, W.; Saputro, I. E.; Palma, M.; et al.
FOOD CHEMISTRY Volume: 169 Pages: 141-149 Published: FEB 15 2015
7.
Negative pressure cavitation-microwave assisted preparation of extract of Pyrola incarnata Fisch. rich in hyperin, 2 '-O-
galloylhyperin and chimaphilin and evaluation of its antioxidant activity
By: Yao, Xiao-Hui; Zhang, Dong-Yang; Luo, Meng; et al.
FOOD CHEMISTRY Volume: 169 Pages: 270-276 Published: FEB 15 2015
http://www.uni-graz.at/~kappeco/index.htm
Enhanced Deprotection, Coupling, and Cleavage Reactions
Galanin Synthesis
Reaction Reagents Time Max Temp.
(C)
Deprotection 20% Piperidine / DMF 3 min 21=A, 75=B
Coupling HBTU/HOBt/DIEA 0.9/1/1 ,
x10 excess
4 min 21=A, 75=B
Cleavage Reagent K
18 min 38=A and B
GWTLNSAGYLLGPQQFFGLM-NH2 Conditions
Scale: 0.10mmol w/ MBHA Rink Amide Resin, 0.59meq/g. (Novabiochem)
A= Conventional
B= Microwave
GWTLNSAGYLLGPQQFFGLM-NH2
Conventional
(Purity = < 10 %)
Microwave
(Purity = 84.8%)
Efekty nietermiczne?
czy rnice w:
szybkoci
wydajnoci
selektywnoci
to tylko wynik szybkiego, rwnomiernego
ogrzania reagentw?
czy w ogle s rnice?
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ania
olejowa
reaktor
mikrofalowy
Img_8960.jpg
Natalia Wisowska, 2006.
Termostat Obserwacja Palladium Catalyzed Aminocarbonylation of Aryl
Halides
Carbonylation reactions those which incorporate CO
into a molecule often pose experimental challenges
due to the difficulties which accompany the use of
carbon monoxide gas at elevated pressure. In situ
generation of CO gas from reaction of potassium tert-
butoxide and dimethylformamide provides a safe and
convenient route for carbonylation reactions. The
microwave assisted, palladium catalyzed
aminocarbonylation of aryl halides with in situ
generated carbon monoxide has been reported.2 With
the Discover SP camera, both color change and
continued generation of carbon monoxide gas can be
observed throughout the reaction, assisting with rapid
reaction optimization.
1) Leadbeater, N. E.; McGowan, C. C. Clean, Fast Organic Chemistry; CEM Publishing, 2006.
(2) Wan, Y.; Alterman, M.; Larhed, M.; Hallberg, A. J. Org. Chem. 2002, 67, 6232.
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Praktyka
dobr rozpuszczalnika
monitorowanie reakcji
dobr reagentw
wydzielanie produktw (SP)
dodatkowe efekty?