Related Products of 31599-60-7, A common heterocyclic compound, 31599-60-7, name is 1-Iodo-2,3-dimethylbenzene, molecular formula is C8H9I, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
5-{ [6-(l -Methyl- lH-pyrazoI-4-yl)pyridin-3-yl]methyl}-2)5-dihydro-3H-pyrazolo[4,3-c]pyrido[3,2-e]pyridazin-3- one (50 mg, 0.14 mmol), copper(I) iodide (27 mg, 0,14 mmol, 1 equiv), potassium phosphate (0.18 g, 0.84 mmol, 6 equiv), (+/-)-fmr¡ã-Lambdar,Lambda/”-bismethyl-l,2-cyclohexanediamine (59 mg, 0.42 mmol, 3 equiv) and 3-iodo-ortf¡ã-xylene (59 muL, 0.42 mmol., 3 equiv) were combined in degassed NjjV-dimethylformamide (2.5 mL) and placed into an oil bath preheated to 110 0C for 30 minutes. The mixture was cooled to ambient temperature, poured into sodium bicarbonate (25 mL, aqueous saturated) and extracted with ethyl acetate (3 X 50 mL). The combined organic extracts were dried with sodium sulfate, filtered and concentrated in vacuo. The residue was purified by silica gel gradient chromatography (100:0 to 0: 100; hexanes : ethyl acetate containing 10% methanol), providing the titled compound: .H-NMR (400 MHz, CDCl3) delta 8.83 (IH, d, J = 2.2 Hz), 8.78 (IH5 dd, J = 4.6, 1.7 Hz), 8.54 (IH, dd, J = 8.0, 1.9 Hz), 7.92 (IH, dd, J – 7.9, 2.2 Hz), 7.91 (IH, s)? 7,89 (IH, s), 7.51 (IH, dd, J= 8.0, 4.6 Hz), 7.41 (IH, d, J= 8.3 Hz), 7.26 (IH, br s), 7.23-7.21 (2H, m), 5.96 (2H, s), 3.94 (3H, s), 2.36 (3H, s), 2.16 (3H, s) ppm; high resolution mass spectrometry (ES+) m/z 463.1986 [(M+H)+; calculated for C26H23N8O: 463.1989
The synthetic route of 31599-60-7 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; MERCK SHARP &; DOHME CORP.; BESHORE, Douglas, C.; KUDUK, Scott, D.; WO2010/123716; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com