All the chemicals and reagents were purchased from Merck, CDH, Sigma Aldrich, Spectro chem., Loba chem., India and utilized without additional purification. Biotage Microwave Synthesizer (Model: Initiator) was used for carrying out the reactions operating at 150 °C, with the microwave power maximum level of 400 W. 1H NMR and 13C NMR (75 MHz) spectra were recorded using JEOL (300 MHz) NMR spectrometer. The spectra were determined in DMSO-d6 relative to TMS (0.00 ppm). Chemical shifts were reported in δ values utilizing tetramethylsilane as an internal standard with the number of protons, multiplicities (s-singlet, d-doublet, t-triplet, q-quartet, m-multiplet, dd-double doublet) and coupling constants (J) in Hz (Hertz) in 1H NMR. Melting points were determined in open capillaries and were uncorrected.
Microwave synthesizer
Manufactured by Biotage
The Biotage microwave synthesizer is a lab equipment designed for chemical synthesis. It utilizes microwave technology to efficiently heat and accelerate chemical reactions. The core function of this product is to provide a controlled and consistent heating environment for carrying out various chemical processes.
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Lab products found in correlation
3 protocols using microwave synthesizer
1
Microwave Synthesis of Novel Heterocycles
2
Microwave-Assisted Deuteration of 3-Fluoro-4-Aminopyridine
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A solution of 3-fluoro-4-aminopyridine (2) (56 mg, 0.5 mmol) in deuterium oxide (D 2 O) (1.0 ml) in the presence of deuterium chloride (DCl) (37% in D 2 O, 1.0 ml) was irradiated in a sealed Biotage microwave tube at 170°C for 12 hours (hold time) using Biotage microwave synthesizer (maximum pressure 12 bar) by moderation of the initial microwave power (400 W). The mixture was cooled in a stream of compressed air and neutralized with aqueous NaOH solution (5 M, 2.5 ml). The solvent (water) was evaporated under reduced pressure, and the residue was redissolved with CH 2 Cl 2 (3 × 2 ml). The combined organic solution was dried over magnesium sulfate, filtered, and evaporated under reduced pressure to give deuterated isotopologue 3-fluoro-4aminopyridine-5-d 1 (5-d 1 -3F4AP, 2-d 1 ) in 77% yield. 1 H NMR (300 MHz, CDCl 3 ): δ 8.15 (s, 0.95 H), 7.99 (s, 0.97 H), 6.62 (dd, J = 7.0, 5.7 Hz, 0.05 H), 4.07 (br, 2 H) ppm (Supplemental Fig. 1). 13 C NMR (75 MHz, CDCl 3 ): δ 149.21 (d, J C-F = 246.2 Hz), 146.14, 146.04 (d, J C-F = 4.8 Hz), 141.44 (d, J C-F = 10.6 Hz), 136.60 (d, J C-F = 20.1 Hz), 110.90 (d, J C-F = 2.0 Hz), 110.63 (td, J C-D = 24.7 Hz, J C-F = 1.9 Hz) ppm (Supplemental Fig. 2). 19 F NMR (282 MHz, CDCl 3 ): δ -152.3 ppm (Supplemental Fig. 3
3
Synthesis of Deuterated 3-Fluoro-4-Aminopyridine
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A solution of 3-fluoro-4-aminopyridine-5-d 1 (5-d 1 -3F4AP, 2-d 1 ) (18 mg, 0.2 mmol) in D 2 O (1.0 ml) was irradiated in a sealed Biotage microwave tube at 190°C for 8 hours (hold time) using Biotage microwave synthesizer (maximum pressure 12 bar) by moderation of the initial microwave power (400 W). The mixture was cooled in a stream of compressed air, then acidified with 1.0 ml HCl (1 M in aqueous) and neutralized with aqueous NaOH solution (1 M, 1.0 ml). The solvent (water) was evaporated under reduced pressure, and the residue was redissolved with CH 2 Cl 2 (3 × 2 ml). The combined organic solution was dried over magnesium sulfate, filtered, and evaporated under reduced pressure to give deuterated isotopologue 3-fluoro-4aminopyridine-2,5,6-d 3 (2,5,6-d 3 -3F4AP, 2-d 3 ) in 76% yield. 1 H NMR (300 MHz, CDCl 3 ): δ 8.12 (s, 0.02 H), 7.97 (s, 0.07 H), 6.61 (d, J = 7.6, 0.03 H), 4.59 (br, 2 H) ppm (Supplemental Fig. 7). 116.0698, found: 116.0696, 87.1%; C 5 H 4 D 2 FN 2 + : 115.0635, found: 115.0634, 13.1%.
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