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CAS No. : | 4105-21-9 | MDL No. : | MFCD00219254 |
Formula : | C13H10N2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | KDHWCFCNNGUJCP-UHFFFAOYSA-N |
M.W : | 194.23 | Pubchem ID : | 201136 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
68% | With tricyclohexylphosphine tetrafluoroborate; palladium diacetate; potassium carbonate; trimethylpyruvic acid; In N,N-dimethyl acetamide; at 100℃; for 12h;Inert atmosphere; | Compound was obtained following the representative procedure, using 2-phenylimidazo[1,2-a]pyridine 2 (300 mg, 1.5 mmol, 1 equiv), <strong>[3032-81-3]1,3-dichloro-5-iodobenzene</strong> (410 mg, 1.5 mmol, 1 equiv) and heating for 12 h. The crude product was purified by silica gel chromatography using dichloromethane as eluent and trituration with methanol afforded 3-(3,5-dichlorophenyl)-2-phenylimidazo[1,2-a]pyridine 19 as a white powder (347 mg, 68percent yield). Rf = 0.60 (petroleum ether/EtOAc: 7/3); Mp = 210-211 °C. 1H NMR (400 MHz, DMSO-d6): delta 8.19 (d, 1H, 3J = 6.8 Hz, H5), 7.84 (t, 1H, 4J = 1.6 Hz, He), 7.73 (d, 1H, 3J = 9.2 Hz, H8), 7.65 (d, 2H, 4J = 1.6 Hz, Hd), 7.61 (d, 2H, 3J = 7.2 Hz, Ha), 7.42-7.32 (m, 4H, H7, Hb and Hc), 6.98 (dd, 1H, 3J = 3J' = 6.8 Hz, H6). 13C NMR (100 MHz, DMSO-d6): delta 144.55 (C), 142.40 (C), 135.27 (2C-Cl), 133.86 (C), 133.16 (C), 129.61 (2Cd), 128.87 (Ce), 128.64 (2Cb), 127.96 (Cc), 127.85 (2Ca), 125.96 (C7), 124.43 (C5), 118.18 (C), 117.05 (C8), 113.16 (C6). IR (KBr) cm-1: 3036 (nuC-Har), 1590, 1560 (nuC=C and nuC=N), 776, 750 (nuC-Cl). MS (ESI) m/z (percent): 339.0 (100) [M + H]+, 341.0 (80) [M + H + 2]+, 343.0 (15) [M + H + 4]+. Anal. Calcd for C19H12Cl2N2: C, 67.27; H, 3.57; N, 8.26. Found: C, 67.50; H, 3.23; N, 7.98. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
87% | With tetrabutylammomium bromide; palladium diacetate; potassium carbonate; 4,5-bis(diphenylphos4,5-bis(diphenylphosphino)-9,9-dimethylxanthenephino)-9,9-dimethylxanthene; In N,N-dimethyl acetamide; water; at 150℃; for 24h; | In a 10 ml flask,Add the magnet,2-phenylimidazo [1,2-a] pyridine (0.3 mmol) was added,<strong>[54439-75-7]2-<strong>[54439-75-7]chloro-4-methoxybenzaldehyde</strong></strong> (0.9 mmol)Potassium carbonate (0.9 mmol),Tetrabutylammonium bromide (0.9 mmol),Palladium acetate (5 molpercent),4,5-bis (diphenylphosphino) -9,9-dimethylXanthene (10molpercent),N, N-dimethylacetamide (4 mL),Water (0.1 mL).The reaction mixture was reacted at 150 ° C for 24 hours,Cooled to room temperature,An appropriate amount of water was added and extracted three times with ethyl acetate,Combine organic phase,Dried over anhydrous magnesium sulfate,Concentrated by filtration, concentrated column chromatography,Separated product 85mg,Yield 87percent. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
78% | With ammonium iodide; water; acetic acid; dimethyl sulfoxide; at 110℃; for 6h;Green chemistry; | General procedure: N-heteroarene (0.25 mmol), diorganyl dichalcogenide (0.125 mmol) NH4I (0.025 mmol, 10 molpercent, 3.6 mg), acetic acid (1 eq.) and the mixture of DMSO/H2O (2.5:2.5 eq.) were placed into a round-bottom flask. The reaction was stirred at 110 °C in an oil bath for appropriate time (Tables 3-6). After the completion of the reaction, the mixture was cooled to room temperature, quenched with water and the aqueous layer was extracted with EtOAc. The organic phase was dried over MgSO4, filtered, and the volatiles were completely removed under vacuum to give the crude product. Purification by flash chromatography on silica with a mixture of Hexane/EtOAc as eluent furnished the desired chalcogenated product. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
84% | With potassium permanganate; di-tert-butyl peroxide; sodium t-butanolate; at 130℃; for 8h; | The preparation method comprises the following steps: adding 0.1 mmol of 2-phenylimidazo[1,2-a]pyridine compound to a 35 mL high pressure tube under an air atmosphere.0.2 mmol of <strong>[1869-24-5]2-(trifluoromethyl)benzenesulfonamide</strong>,0.2 mmol of di-tert-butyl peroxide, 0.1 mmolPotassium permanganate, 0.1 mmol of sodium t-butoxide, hexafluoroisopropanol and methanol (volume ratio 1:9) 2 mL, reacted at 130 C for 8 hours;After completion, chromatographic separation (silica gel 200-300 mesh, eluent: ethyl acetate / petroleum ether gradient elution, ratio from 0/100 to100/0), dried to a yellow solid, yield 84%. |