Cavity, microwave

In plasma chemical vapor deposition (PCVD), the starting materials are typically SiCl, O2, 2 6 GeCl (see Plasma technology). Plasma chemical vapor deposition is similar to MCVD in that the reactants are carried into a hoUow siUca tube, but PCVD uses a moving microwave cavity rather than a torch. The plasma formed inside the microwave cavity results in the deposition of a compact glass layer along the inner wall of the tube. The temperatures involved in PCVD are lower than those in MCVD, and no oxide soots are formed. Also, the PCVD method is not affected by the heat capacities or thermal conductivities of the deposits. 

For electron spin resonance (ESR) measurements, the sample is placed in a resonant microwave cavity between the pole pieces of an electromagnet. The magnetic field is gradually increased, which induces a Zeeman splitting of the excila-... 

Entirely different factors have to be considered when the electrochemical cell is placed in a microwave cavity [Fig. 4(b)]. Only a very small volume of water can be introduced into the cavity without drastically... 

Figure4b. Cell in microwave cavity (l)resonator, (2) waveguide, (3) cylindrical exit, (4) electrochemical cell, (5) working electrode, (6) electrolyte, (7) counter-electrode, (8) contact wire to working electrode, (9) opical light guide.

Another series of pyrroles, structurally related to amino acids, was obtained in a microwave-assisted solvent-free condensation of a-amino acid methyl esters with chloroenones, which provided the four-carbon unit of the pyrrole. The reaction was carried out by mixing the reagents on silica gel and irradiating for 2-6 min inside a multimode microwave cavity (Scheme 7). The authors reported higher yields and cleaner products when microwaves were used instead of conventional heating [34],... 

A similar deposition system uses a plasma which is produced by a traveling microwave cavity. No other source of heat is required. The deposition system is shown schematically in Fig. 16.12. The reactants are the same as in the thermal CVD process. Pressure is maintained at approximately 1 Torr. In this case, the deposition occurs at lower temperature, no soot is formed and a compact glass is produced directly. A main advantage of this method is the more accurate grading of the refractive index of the cladding material. 

Figure 3.15 Schematic diagram of the Hewlett-Packard 5921A GC-AED system and cutaway view of the microwave cavity. (Adapted with permission from ref. 202 and 203. Copyright Dr. Alfred Huethig Publishers and American Chemical Society).

The resonant microwave frequency reaching the sample is determined by the effective length of the microwave cavity. The actual length is somewhat... 

In a microwave cavity containing an ionized gas, the resonant frequency shifts in proportion to the electron density n (Slater, 1946). This effect has been used by Warman and Sauer (1970, 1975) to measure n as a function of time... 

Shimamori and Hatano (1976) describe a Febetron-injected microwave cavity apparatus for measuring electron concentration following pulse irradiation. Its application to thermalization in Ar and CH4 is similar to the method of Warman and Sauer (1975). In a related experiment, Hatano et al. (private communication) measure the electron collision frequency directly. 

This chapter provides a detailed description of the various commercially available microwave reactors that are dedicated for microwave-assisted organic synthesis. A comprehensive coverage of microwave oven design, applicator theory, and a description of waveguides, magnetrons, and microwave cavities lies beyond the scope of this book. Excellent coverage of these topics can be found elsewhere [1—4]. An overview of experimental, non-commercial microwave reactors has recently been presented by Stuerga and Delmotte [4],... 

An example of solid-phase microwave synthesis where the use of open-vessel technology is essential is shown in Scheme 4.10. The transesterification of /3-keto esters with a supported alcohol (Wang resin) is carried out in 1,2-dichlorobenzene (DCB) as a solvent under controlled microwave heating conditions [22], The temperature is kept constant at 170 °C, ca. 10 degrees below the boiling point of the solvent, thereby allowing safe processing in the microwave cavity. In order to achieve full conversion to the desired resin-bound /3-keto ester, it is essential that the methanol formed can be removed from the equilibrium [22]. 

As already mentioned above, a different strategy to achieve high throughput in microwave-assisted reactions can be realized by performing automated sequential microwave synthesis in monomode microwave reactors. Since it is currently not feasible to have more than one reaction vessel in a monomode microwave cavity, a robotic system has been integrated into a platform that moves individual reaction... 

One major benefit of performing microwave-assisted reactions at atmospheric pressure is the possibility of using standard laboratory glassware (round-bottomed flasks, reflux condensers) in the microwave cavity to carry out syntheses on a larger scale. In contrast, pressurized reactions require special vessels and scale-up to more... 

The reactions were carried out in sealed Pyrex tubes employing a prototype single-mode microwave cavity. The reagents were added to the resin-bound aryl halide under a nitrogen atmosphere and irradiated for the time periods indicated (Scheme 7.14). Rather short reaction times provided almost quantitative conversions, with minimal degradation of the solid support. 

The resin-bound salicylic esters were suspended in N,N-dimethylformamide (DMF) and placed in an Erlenmeyer flask within a domestic microwave cavity. After microwave irradiation for 4—6 min (1 min cycles), the reaction mixture was allowed to cool to ambient temperature and the resin was collected by fdtration and washed with methanol and dichloromethane. The desired compounds were subsequently cleaved with trifluoroacetic acid in dichloromethane. Removal of the solvent by evap-... 

For this solid-phase approach, conventional iPrOCH2-functionalized polystyrene resin (Merrifield linker) was employed. After attachment of the requisite substrate, the resin was pre-swollen in a solution of barium(II) hydroxide in N,N-dimethyl-formamide within an appropriate sealed microwave vial. The vial was heated in the microwave cavity for 5 x 2 min cycles (overall 10 min) with the reaction mixture being allowed to cool to room temperature in between irradiation cycles (Scheme 7.50), leading to comparatively modest isolated yields of hydantoins. 

The isocyanates were added to the respective resin-bound amines suspended in dichloromethane in open glass tubes. The resulting reaction mixtures were each irradiated in a single-mode microwave cavity for 2 min intervals (no temperature measurement given) (Scheme 7.52). After each step, samples were collected for on-bead FTIR analysis. Within 12 min (six irradiation cycles), each reaction had reached completion. Acid cleavage of the polymer-bound ureas furnished the corresponding hydrouracils. 

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