Microwave Assisted Organic Synthesis 2005
DOI: 10.1002/9781444305548.ch9
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Scale‐Up of Microwave‐Assisted Organic Synthesis

Abstract: In 1986 it was first reported that organic reactions could be conducted by heating in sealed containers in domestic microwave ovens 1,2 . Rate enhancements of up to three orders of magnitude were disclosed 3 . However, temperature and pressure measurement were technically difficult to achieve and in some instances the vessels deformed or exploded 1-3 .From these publications, workers interested in exploring the microwave technique perceived it to be simultaneously beneficial through increased rates, yet hazard… Show more

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Cited by 15 publications
(12 citation statements)
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References 107 publications
(151 reference statements)
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“…This may have occurred in part through perceived limitations of the technique as discussed below, but not entirely. Different perspectives of chemists and chemical engineers in chemical discovery and manufacturing respectively, also may have had an influence . A limited knowledge of the reaction conditions may be sufficient to enable synthetic chemists to obtain a desired product in the laboratory.…”
Section: Discussionmentioning
confidence: 99%
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“…This may have occurred in part through perceived limitations of the technique as discussed below, but not entirely. Different perspectives of chemists and chemical engineers in chemical discovery and manufacturing respectively, also may have had an influence . A limited knowledge of the reaction conditions may be sufficient to enable synthetic chemists to obtain a desired product in the laboratory.…”
Section: Discussionmentioning
confidence: 99%
“…The time might seem ideal for scaling up capacity for microwave reactions by at least an order of magnitude above the kilogram level. Doubts have been expressed, however, that scale up may not be feasible owing to insufficient depth of penetration of microwaves, ,,, heating rates being too slow to offer advantages, the cost of generating microwave energy being too high, , and the significant engineering challenges associated with safely heating reactions under pressure in large, microwave-transparent vessels …”
Section: Discussionmentioning
confidence: 99%
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“…With reference to the successful small-scale examples, the larger scale microwaveassisted synthesis technology that can economically provide product on a multikilogram scale (or even higher) need to be developed for making it to become widespread technology in the future. Actually, for the ability of the direct homogenous heating of the reaction mixtures under microwave irradiation to facilitate direct scaling without heat and mass transport issues [7], several reports have demonstrated the feasibility of direct scaling reaction conditions from small-scale single-mode (0.5-5 mL) to larger scale batch modes (10-500 mL), such as multimode [8][9][10][11][12][13][14], monomode [15,16] and continuous-flow microwave reactors [17][18][19][20], without reoptimization of the reaction conditions. The larger scale microwave-assisted polymerizations (250-400 mL) have also been performed in domestic microwave ovens that equipped with reflux condensers [21,22].…”
Section: Introductionmentioning
confidence: 99%
“…We thus have examined microwave heating as a simpler, more readily available methodology for activating the solid. [6][7][8] We have tested this idea on the extensively studied Diels-Alder reaction [9][10][11][12][13][14][15][16] and Claisen rearrangement. [17][18][19][20][21][22][23] We have previously examined in detail the Diels-Alder reaction on thermally activated alumina, [24][25][26][27][28][29][30] but the Claisen rearrangement is new to us.…”
mentioning
confidence: 99%