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Initiator 2

Manufactured by Biotage
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Sourced in Sweden

The Biotage Initiator 2.0 is a microwave synthesis system designed for organic and medicinal chemistry applications. It provides controlled microwave heating to facilitate chemical reactions and transformations.

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Lab products found in correlation

Apex qe instrument, by Bruker (3 mentions) Iraffinity 1, by Shimadzu (3 mentions) Vance 400 mhz spectrometer, by Bruker (2 mentions) Ft ir spectrometer, by Shimadzu (1 mentions) Isolera prime, by Biotage (1 mentions)

9 protocols using initiator 2

1

Microwave-Assisted Extraction of Plant Material

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Raw material (500 mg) was suspended in 20 mL of 60% MeOH in water in a glass, sealed vial using an automatic Biotage Initiator™ 2.0 (Uppsala, Sweden; 2.45 GHz high-frequency microwaves; power range: 0–300 W). Settings were as follows: temperature thermostatically kept at 80 °C; power: 60 W; extraction time: 5 min. The resulting suspension was filtered and freeze-dried.
Della Valle A., Dimmito M.P., Zengin G., Pieretti S., Mollica A., Locatelli M., Cichelli A., Novellino E., Ak G., Yerlikaya S., Baloglu M.C., Celik Altunoglu Y, & Stefanucci A. (2020). Exploring the Nutraceutical Potential of Dried Pepper Capsicum annuum L. on Market from Altino in Abruzzo Region. Antioxidants, 9(5), 400.
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2

Microwave-assisted Organic Synthesis Protocols

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All microwave reactions were conducted using the single-mode Biotage Initiator 2.0 (Biotage, Uppsala, Sweden); all the products were characterized by spectral data (HR-ESI-MS, 1H-NMR, 13C-NMR, FT-IR). 1H- and 13C-NMR spectra (400 MHz for proton and 100 MHz for carbon) were obtained on a Bruker-Vance 400 MHz spectrometer (Bruker, Rheinstetten, Germany), using CDCl3 and DMSO-d6 as solvents. Tetramethylsilane was used as an internal standard. Data for 1H-NMR are reported as follows: chemical shifts (δ ppm), multiplicity (s, singlet; d, doublet; dd, doublet of doublets; t, triplet; m, multiplet), integration and coupling constant (Hz). Chemical shifts (δ) and J values are reported in ppm and Hz, respectively, relative to the solvent peak CDCl3 at 7.2 ppm for protons and 77 ppm for carbon atoms. NMR Spectra were analyzed using MestReNova software (version 10, Mestrela research, Feliciano Barrera-Bajo, Spain). The IR spectrum was obtained using FT-IR spectrometer (Shimadzu, IRAffinity-1S, and Columbia, MD, USA). High-resolution ESI-MS was acquired with a Bruker Apex-Qe instrument. Melting points (uncorrected) were measured on a Fisher-Jones melting point apparatus. All reagents and chemicals were obtained from Aldrich Chemical Company (St. Louis, MO, USA) and Alfa Aesar (Ward Hill, MA, USA) and were used without further purification.
Abebe F., Sutton T., Perkins P., Makins-Dennis K, & Winstead A. (2018). Microwave-assisted synthesis of rhodamine derivatives. Green chemistry letters and reviews, 11(3), 237-245.
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3

Microwave-assisted Organic Synthesis Protocols

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All microwave reactions were conducted using the single-mode Biotage Initiator 2.0 (Biotage, Uppsala, Sweden); all the products were characterized by spectral data (HR-ESI-MS, 1H-NMR, 13C-NMR, FT-IR). 1H- and 13C-NMR spectra (400 MHz for proton and 100 MHz for carbon) were obtained on a Bruker-Vance 400 MHz spectrometer (Bruker, Rheinstetten, Germany), using CDCl3 and DMSO-d6 as solvents. Tetramethylsilane was used as an internal standard. Data for 1H-NMR are reported as follows: chemical shifts (δ ppm), multiplicity (s, singlet; d, doublet; dd, doublet of doublets; t, triplet; m, multiplet), integration and coupling constant (Hz). Chemical shifts (δ) and J values are reported in ppm and Hz, respectively, relative to the solvent peak CDCl3 at 7.2 ppm for protons and 77 ppm for carbon atoms. NMR Spectra were analyzed using MestReNova software (version 10, Mestrela research, Feliciano Barrera-Bajo, Spain). The IR spectrum was obtained using FT-IR spectrometer (Shimadzu, IRAffinity-1S, and Columbia, MD, USA). High-resolution ESI-MS was acquired with a Bruker Apex-Qe instrument. Melting points (uncorrected) were measured on a Fisher-Jones melting point apparatus. All reagents and chemicals were obtained from Aldrich Chemical Company (St. Louis, MO, USA) and Alfa Aesar (Ward Hill, MA, USA) and were used without further purification.
Abebe F., Sutton T., Perkins P., Makins-Dennis K, & Winstead A. (2018). Microwave-assisted synthesis of rhodamine derivatives. Green chemistry letters and reviews, 11(3), 237-245.
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4

Microwave-Assisted Synthesis of Biguanide Derivatives

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Biguanide derivatives were prepared by modifying a procedure reported in the literature.19 The amine derivative (0.82–2.4 mmol) was added to a solution of dicyandiamide (1.0 eq) in 2.4–3.7 mL of dry CH3CN, and TMSCl (1.1 eq) was slowly added dropwise to the mixture. The mixture was stirred and irradiated with adjustable power in the range of 0–400 W, at 2.45 GHz for 10 or 15 minutes at 130°C or 150°C using a microwave reactor (Biotage® Initiator 2.0; Biotage AB, Uppsala, Sweden). After the mixture was cooled down to approximately 50°C, isopropyl alcohol (iPrOH) (3.0 eq) was added slowly, and the mixture was further stirred and irradiated at 125°C for 1 minute. The precipitation of the biguanide hydrochloride salt was washed twice with CH3CN. The preparation of compound 1 was included in Supplementary material.
Narise K., Okuda K., Enomoto Y., Hirayama T, & Nagasawa H. (2014). Optimization of biguanide derivatives as selective antitumor agents blocking adaptive stress responses in the tumor microenvironment. Drug Design, Development and Therapy, 8, 701-717.
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5

Microwave-Assisted Extraction of Saffron

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Dried samples were ground manually in a mortar and sifted to obtain a uniform granulometry before performing the extraction. MAE was carried out by an automatic Biotage Initiator 2.0 (Uppsala, Sweden; 2.45 GHz high-frequency microwaves, power range: 0–300 W). The internal vial temperature was controlled by an infra-red sensor probe. Manually ground saffron (10 mg) was placed in a 10 mL sealed vessel, suitable for an automatic single-mode microwave reactor, and 0.8 mL of deuterated methanol (CD3OD, 99.8 atom% of deuterium, Euriso-Top, France) was added to the sample to form a yellow–orange suspension. The sample was heated by microwave irradiation for 30 min at 40 °C, followed by cooling with pressurized air. An internal standard (3-(trimethylsilyl)-propionic-2,2,3,3-d4 acid sodium salt, TSP, 1 mM) was added, and the suspension was stirred magnetically for 1 min in the dark. The liquid phase was carefully separated from the solid precipitate and directly analyzed by NMR [9 (link)].
Samaha H., Chahine N., Sobolev A.P., Menghini L, & Makhlouf H. (2021). 1H-NMR Metabolic Profiling and Antioxidant Activity of Saffron (Crocus sativus) Cultivated in Lebanon. Molecules, 26(16), 4906.
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6

Synthesis and Characterization of Novel Compound

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All the reagents and solvents were purchased as analytical-grade and used without further purification unless otherwise stated. The stock solutions of metal ions were prepared from their nitrate and chloride salts and anion species from their tetrabutylammonium salts. Distilled deionized water was used throughout the experiments. 1H-NMR and 13C-NMR spectra were recorded using an Avance 400 MHz spectrometer (Bruker Billerica, Karlsruhe, Germany) with tetramethylsilane (TMS) as internal standard and deuterated chloroform (CDCl3) as solvent. NMR spectra were analyzed using MestReNova software (version 10, Mestrela Research, Feliciano Barrera-Bajo, Spain). The IR spectrum was obtained using FT-IR spectrometer (Shimadzu, IRAffinity-1S, Columbia, MD, USA). High resolution electrospray ionization mass spectrometry (ESI-MS) was acquired with a Bruker Apex-Qe instrument. All UV-vis spectroscopy experiments were recorded using a Cary UV/vis spectrophotometer 5000 (Varian, Walnut Creek, CA, USA). Fluorescence emission spectra experiments were measured using a Cary 60 series spectrometer (Agilent, Walnut Creek, CA, USA), with excitation and emission slit widths of 5 nm and excitation wavelength at 510 nm. MAOS reactions were carried out in a single mode Biotage Initiator 2.0 (Biotage, Uppsala, Sweden).
Abebe F., Sutton T., Perkins P, & Shaw R. (2018). Two colorimetric fluorescent turn-on chemosensors for detection of Al3+and N3−: Synthesis, photophysical and computational studies. Luminescence : the journal of biological and chemical luminescence, 33(7), 1194-1201.
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7

Microwave-Assisted Synthesis of Trisubstituted Pyridines

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To a microwave vial under argon containing substituted 4-bromopyridine (0.5 mmol), the corresponding boronic acid (0.51 mmol) and Pd(PPh3)4 (0.02 mmol) were dissolved in anhydrous THF (3.5 mL), and were stirred at room temperature for 10 min. Then, a solution of 0.5 mL KOH (1 M) was added to the mixture. The mixture was heated at 130 °C for 11 min in a microwave oven (Biotage Initiator 2.5). The solvent was removed under vacuum to yield a black residue, which was dissolved in 20 mL of CH2Cl2 and washed with 10 mL of water. The aqueous phase was extracted with CH2Cl2 (2 × 20 mL). The combined organic phases were washed with brine (20 mL), dried over Na2SO4, filtered, and concentrated to dryness. Flash chromatography in CH2Cl2:hexane in a 1:1 ratio yielded the corresponding trisubstituted 2,4,6-pyridine compounds.
Gamonal Ruiz-Crespo A., Galán-Fernández L., Martínez-Martín P, & Rodríguez-Ubis J.C. (2022). An Orthogonal Synthetic Approach to Nonsymmetrical Bisazolyl 2,4,6-Trisubstituted Pyridines. Molecules, 27(5), 1746.
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8

Optimized Microwave-Assisted Organic Synthesis

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All starting materials and reagents were purchased from commercially available sources and used without further purification, with the exception of THF, which was purified on a solvent purification system prior to the reaction. 1H NMR shifts are measured using the solvent residual peak as the internal standard (CDCl3δ 7.26, THF-d8δ 3.58), and reported as follows: chemical shift, multiplicity (s = singlet, br s = broad singlet, d = doublet, t = triplet, p = pentet, dd = doublet of doublets, hept = heptet, q = quartet, m = multiplet), coupling constant (Hz), and integration. Microwave reactions were performed via the Biotage Initiator 2.5. Purification via column chromatography was performed on the Biotage Isolera Prime, with Biotage SNAP 12 g C18 cartridges, in a solvent system of acetonitrile (MeCN) and water (H2O), with each containing 0.05% trifluoroacetic acid (TFA). Column gradients are measured in terms of column volumes (CV). Other abbreviations used: THF = tetrahydrofuran; DMF = dimethylformamide; DMSO = dimethyl sulfoxide; HATU = 1-[bis(dimethylamino)methylene]-1H-1,2,3-triazolo[4,5-b]pyridinium 3-oxide hexafluorophosphate.
Gazquez Casals A., Berkowitz A.J., Yu A.J., Waters H.E., Schiavone D.V., Kapkayeva D.M., Morrison L.A, & Murelli R.P. (2023). Antiviral activity of amide-appended α-hydroxytropolones against herpes simplex virus-1 and -2. RSC Advances, 13(13), 8743-8752.
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9

Microwave-Assisted Synthesis of 3-Methoxycarbonyl Indazole Derivative

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To a microwave vial under argon contained substituted monofluorinated 4-bromopyridine (1 eq.), 3-methoxycarbonyl indazole (1.2 eq.), K2CO3 (1.2 eq.), and dry recently distilled DMF (3 mL). The mixture was stirred at room temperature for 2 min and then heated at 140 °C for 2 h in a microwave oven (Biotage Initiator 2.5). The reaction mixture was poured on 15 mL of water and the resulting solid was isolated by centrifugation and washed 3 times with 10 mL of water. The product was purified by Flash chromatography in CH2Cl2:MeOH in a 95:5.
Gamonal Ruiz-Crespo A., Galán-Fernández L., Martínez-Martín P, & Rodríguez-Ubis J.C. (2022). An Orthogonal Synthetic Approach to Nonsymmetrical Bisazolyl 2,4,6-Trisubstituted Pyridines. Molecules, 27(5), 1746.
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