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Microwave reactor

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The Microwave reactor is a laboratory instrument designed to facilitate chemical reactions using microwave energy. It provides a controlled environment for heating and stirring reactions, enabling efficient and consistent sample processing.

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Lab products found in correlation

1100 system, by Agilent Technologies (1 mentions) Combiflash companion system, by Teledyne (1 mentions) Api 150ex mass spectrometer, by Agilent Technologies (1 mentions) Eclipse xdb c18 column, by Agilent Technologies (1 mentions) 1200 hplc system, by Agilent Technologies (1 mentions)

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Initiator+ microwave reactor

6 protocols using microwave reactor

1

Microwave-assisted Photocatalyst Synthesis

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The photocatalysts were prepared in a one-step microwave process as follows: 2 mmol of bismuth nitrate and 1 mmol of sodium tungstate were added to a mixture solution with a certain proportion of EA and water, stirring evenly. The total volume of EA (99%) and water remained 6 ml. The mixed solution was then transferred to a microwave reactor (Biotage Sweden) at 434 K, and the synthetic reaction was performed for 10 min. The resulting samples were received after centrifugal washing and baking at 354 K for 10 h in the oven. The as-prepared samples are recorded as EA:X, where X is the volume ratio of EA and water.
Liu X., Wang S., Wang S., Shi H., Zhang X, & Zhong Z. (2019). The three-dimensional flower-like Bi2WO6 assisted by ethanolamine through a microwave method for efficient photocatalytic activity. Royal Society Open Science, 6(3), 181422.
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2

Synthesis of 2-Chlorothiazolo[4,5-c]pyridine Derivative

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Example 28

[Figure (not displayed)]

Step A

In a microwave tube commercially available 6-bromo-2-chlorothiazolo[4,5-c]pyridine (50 mg, 0.20 mmol) and morpholine (3.5 mL, 40.1 mmol) were added. The tube was sealed and stirred at room temperature for 10 minutes and then at 150° C. for 10 minutes in a microwave reactor (Biotage). The solvent was removed under reduce pressure to afford the title compound (0.60 g, 78%).

1H NMR (400 MHz, DMSO-d6) δ=8.48 (s, 1H), 8.05 (s, 1H), 3.61 (dd, 4H), 3.17-3.03 (m, 4H).

US11684625B2. Compounds for the treatment, alleviation or prevention of disorders associated with tau aggregates (2023-06-27). AC Immune SA [CH]. Inventors: Sreenivasachary Nampally [CH], Emanuele Gabellieri [CH], Jerome Molette [FR].
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3

Synthesis of Betaine-Functionalized Poly(ethylene boc-aspartate diglyceride)

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B-PED is synthesized according to conditions modified from those previously described29 (link). Briefly, EGDE (1000 mg), Boc-ASP-OH (1338.8 mg), and TBAB (5 mg) were dissolved in 0.6 mL of DMF. The mixture was reacted at 120 °C under N2 for 20 minutes in a microwave reactor (Biotage, Uppsala, Sweden). The resulting intermediate polymer, poly(ethylene boc-aspartate diglyceride) (PED-boc) was solubilized in 2 mL DCM and precipitated into diethyl ether. t-Boc was removed via addition of 4:1 DCM:TFA ([TFA] = 2.5 mM). After 2 hours of stirring at room temperature, solvent was subsequently removed via a rotatory evaporator for 2 hours. Multiple precipitation steps in diethyl ether were used to remove excess reagents, DMF, and TFA. PED was then washed overnight in diethyl ether and dried under vacuum until further use. B-PED was prepared by combining PED (0.108 M of reactive sites), betaine (0.217 M), NHS (0.217 M), DCC (0.260 M), and DMAP (0.011 M) into DMF. The solution was stirred at 30 °C under N2 for 48 hours. An insoluble dicyclohexylurea by-product was removed via centrifugation and filtration (0.22 μm). B-PED was then purified via multiple precipitation steps in diethyl ether, washed in ethanol, and dialyzed against deionized water for 18 hours.
Hwang M.P., Ding X., Gao J., Acharya A.P., Little S.R, & Wang Y. (2018). A Biocompatible Betaine-functionalized Polycation for Coacervation. Soft matter, 14(3), 387-395.
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4

Argon-Atmosphere Microwave-Assisted Synthesis

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All experiments were carried out under an argon atmosphere in flame-dried glassware using standard inert techniques for introducing reagents and solvents, unless otherwise noted. N,N-Dimethylformamide (DMF) was distilled over calcium hydride and stored in a bottle with activated molecular sieves (4 Å). All commercially available materials were used as received without further purification. 1H NMR, 13C NMR and 19F NMR spectra were measured on a JEOL ECZS 400S spectrometer (1H: 400MHz, 13C: 100 MHz, 19F: 376 MHz). Chemical shifts of 1H NMR and 13C NMR are reported in parts per million from tetramethylsilane (TMS), used as an internal standard at 0 ppm. Chemical shifts of 19F NMR are reported in parts per million from trichlorofluoromethane (CFCl3), used as an internal standard at 0 ppm. All dates are reported as follows: chemical shifts, relative integration value, multiplicity (s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet), and coupling constants (Hz). High-resolution mass spectroscopy (HRMS) experiments were performed with a double-focusing mass spectrometer with EI. Melting points were measured on Yanaco melting point apparatus MP-500V without correction. Microwave reactions were performed in microwave tubes with clip lids using a Biotage Initiator microwave reactor.
Ogawa F., Takeda M., Miyanaga K., Tani K., Yamazawa R., Ito K., Tarui A., Sato K, & Omote M. (2017). Development of a fluorogenic small substrate for dipeptidyl peptidase-4. Beilstein Journal of Organic Chemistry, 13, 2690-2697.
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5

Fabrication of Porous PGS Grafts

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PGS infused salt tube was placed in a vacuum oven with gradual heating to 150°C under 30 Torr vacuum for 24 h. Microwave-assisted curing method (mwPGS): Each salt mold loaded with 20 wv% PGS prepolymer solutions in THF was placed in a microwave vial with silica desiccant (approximately 1.5 g per vial) and cured in the microwave reactor (Biotage® Initiator, Charlotte, NC) under varying reaction temperature conditions of 120, 140, 160 and 170°C for 3 h. The reaction temperature was reached through gradual heating at a rate of 10°C/min from the starting temperature of 100°C. After completion of the curing process, salt molds were dissolved in a series of two 10 mL water baths (first bath for 24 h and second bath for 48 h). The final grafts were lyophilized before further examination.
Lee S.H., Lee K.W., Gade P.S., Robertson A.M, & Wang Y. (2017). Microwave-assisted facile fabrication of porous poly (glycerol sebacate) scaffolds. Journal of biomaterials science. Polymer edition, 29(7-9), 907-916.
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6

Characterization of Synthesized Compounds

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Melting points were measured on a SGW X-4 Micro-Melting point detector without correction. The proton nuclear magnetic resonance (1H NMR) spectra were measured on a JNM-ECA-400 (400 MHz) spectrometer using tetramethylsilane (TMS) as internal standard. The solvent used was DMSO unless indicated. Mass spectra (MS) were measured on an API-150EX mass spectrometer with electrospray ionization connected with an Agilent 1100 system. The microwave reactions were performed on a microwave reactor from Biotage, Inc. Thin-layer chromatography (TLC) was performed on silica gel GF254 plates. Silica gel GF254 and H (200–300 mesh) from Qingdao Haiyang Chemical Company was used for TLC and preparative TLC, respectively. Medium-pressure column chromatography was performed using a CombiFlash companion system from ISCO, Inc. to purify target compounds. All chemicals were obtained from Beijing Chemical Works or Sigma-Aldrich, Inc. The purity of target compounds was measured with HPLC methods and reached >95% for biological assays. The HPLC analyses were performed by using an Agilent 1200 HPLC system with a UV detector and an Agilent Eclipse XDB-C18 column (150 mm × 4.6 mm, 5 µm) under the conditions of elution with 35–70% acetonitrile (CAN)) in water, flow rate 0.8 mL/min, UV detection at 254 nm, and injection volume of 15 L.
Wang S.B., Cui M., Wang X.F., Ohkoshi E., Goto M., Yang D.X., Li L., Yuan S., Morris-Natschke S.L., Lee K.H, & Xie L. (2016). Synthesis, Biological Evaluation, and Physicochemical Property Assessment of 4-Substituted 2-phenylaminoquinazolines as Mer Tyrosine Kinase Inhibitors. Bioorganic & medicinal chemistry, 24(13), 3083-3092.
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