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CAS No. : | 133427-08-4 | MDL No. : | MFCD06739251 |
Formula : | C8H6N2O2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | WHOCKNWCRFHEMH-UHFFFAOYSA-N |
M.W : | 162.15 | Pubchem ID : | 11715357 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P280 | UN#: | N/A |
Hazard Statements: | H302-H317 | Packing Group: | N/A |
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 |
---|---|---|
In ethanol; water; for 14h;Reflux; | Example 9: Synthesis of 3-(4-Fluorophenyl)-imidazo[l,2-a]pyridine-8-carboxylic acid (9); Chloroacetaldehyde (45% aqueous solution) (6.6 mL, 38 mmol) is added to the stirred solution of 2-aminonicotinic acid (5.0 g, 25 mmol) in ethanol (35 mL) and warmed at reflux for 14 hours. The reaction mixture is concentrated and the crude material is triturated with EtOH-Et20 to afford imidazo[l,2-a]pyridine-8-carboxylic acid. Mp: 296-299C. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
The solution was concentrated under reduced pressure to remove the methanol, the aqueous solution acidified using 2N hydrochloric acid, and the mixture evaporated under reduced pressure to give the title compound as a yellow solid. 1H-NMR (DMSO-d6, 400 MHz) delta: 7.60 (dd, 1H), 8.10 (s, 1H), 8.41 (d, 1H), 8.55 (s, 1H), 9.18 (d, 1H) LRMS: m/z ES+ 163 [MH]+ | ||
[0310] Lithium hydroxide solution (2.5 mL, 1M in water) was added to a solution of the ester from preparation 8 (400 mg, 2.27 mmol) in methanol (5 mL) and the solution stirred at room temperature for 90 minutes. The solution was concentrated in vacuo to remove the methanol, the aqueous solution acidified using 2M hydrochloric acid, and the mixture concentrated in vacuo to give the title compound as a yellow solid. [0311] 1HNMR (DMSO-D6, 400 MHz): 7.60 (dd, 1H), 8.10 (s, 1H), 8.41 (d, 1H), 8.55 (s, 1H), 9.18 (d, 1H) [0312] MS TSP+ m/z 163 [MH]+ | ||
[0306] [C00009] [00009] [0307] Lithium hydroxide solution (2.5 ml, 1M in water) was added to a solution of the ester from preparation 3 (400 mg, 2.27 mmol) in methanol (5 ml) and the solution stirred at room temperature for 90 minutes. The solution was concentrated in vacuo to remove the methanol, the aqueous solution acidified using 2M hydrochloric acid, and the mixture evaporated under reduced pressure to give the title compound as a yellow solid. [0308] 1H NMR (DMSO-D6, 400 MHz): delta: 7.60 (dd, 1H), 8.10 (s, 1H), 8.41 (d, 1H), 8.55 (s, 1H), 9.18 (d, 1H) [0309] MS TSP+m/z 163 [MH]+ |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
63% | EXAMPLE 1 Syn-Imidazo[1,2-a]Pyridine-8-Carboxylic Acid (4-[2-(2,3-Dihydro-Benzo[b]Thiophen-6-Yloxy)-5-Fluoro-Pyridine-3-Carbonyl]-Amino}-Cyclohexyl)-Amide The amine of preparation 7 (150 mg, 0.39 mmol), the carboxylic acid of preparation 4 (87 mg, 0.43 mmol), 1-hydroxybenzotriazole hydrate (58 mg, 0.43 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (82 mg, 0.43 mmol) and 4-methylmorpholine (47 muL, 0.43 mmol) were dissolved in dichloromethane (20 mL) and the reaction mixture stirred at room temperature for 18 hours. The reaction mixture was concentrated in vacuo and the residue dissolved in N,N-dimethylformamide (10 mL) and stirred at room temperature for 18 hours. The reaction mixture was concentrated in vacuo, the residue partitioned between ethyl acetate (50 mL) and water (30 mL) and the organic layer washed with brine, dried over magnesium sulphate and concentrated in vacuo. The residue was purified by column chromatography on silica gel eluding with pentane:ethyl acetate 85:15 to 0:100. The crude product was purified by column chromatography on silica gel again, eluding with ethyl acetate to yield the title product as a white solid, 130 mg (63%). 1H NMR(CDCl3, 400 MHz): delta: 1.90(m, 8H), 3.30(t, 2H), 3.40(t, 2H), 4.20(m, 1H), 4.30(m, 1H), 6.85(m, 1H), 7.00(t, 1H), 7.05(s, 1H), 7.20(d, 1H), 7.45(s, 1H), 7.65(s, 1H), 8.05(m, 2H), 8.25(m, 2H), 8.35(m, 1H), 10.50(m, 1H) MS ES+m/z 554 [MNa]+ Microanalysis: Observed-C=61.99%, H=4.90%, N=12.86% C28H26FN5O3S Calculated-C=62.00%, H=5.05%, N=12.91% |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With 4-methyl-morpholine; benzotriazol-1-ol; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; In DMF (N,N-dimethyl-formamide); at 20℃; for 18h; | EXAMPLE 6 Syn-<strong>[133427-08-4]Imidazo[1,2-a]pyridine-8-carboxylic acid</strong>(4-[5-fluoro-2-(3-methylsulfanyl-phenoxy)-pyridine-3-carbonyl]-amino}-cyclohexyl)-amide The amine of preparation 18 (250 mg, 0.60 mmol) was dissolved in N,N-dimethylformamide (7 mL) and the solution treated with 1-hydroxybenzotriazole hydrate (84 mg, 0.60 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (124 mg, 0.69 mmol), 4-methylmorpholine (205 muL, 1.88 mmol) and the carboxylic acid of preparation 9 (90 mg, 0.55 mmol). The reaction mixture was stirred at room temperature for 18 hours. The mixture was diluted with ethyl acetate:water 3:1 (28 mL) and the aqueous extracted with ethyl acetate (*2). The organics were washed with 10% citric acid solution (7 mL), saturated sodium hydrogen carbonate solution (7 mL) and brine (7 mL). The organic layers were dried over magnesium sulphate and concentrated in vacuo. The residue was purified by column chromatography on silica gel eluding with pentane:ethyl acetate 70:30 to 20:80 to yield the title product, 80 mg. 1H-NMR(CDCl3, 400 MHz): 1.91(m, 8H), 2.43(s, 3H), 4.23(m, 1H), 4.32(m, 1H), 6.94(m, 2H), 7.06(m, 1H), 7.14(m, 1H), 7.31(m, 1H), 7.37(m, 1H), 7.60(m, 1H), 8.01(m, 1H), 8.06(m, 1H), 8.17(s, 1H), 8.24(d, 1H), 8.36(m, 1H), 10.53(m, 1H). MS ES+ m/z 520 [MH]+ |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In acetonitrile; at 150℃; for 2h;microwave irradiation;Product distribution / selectivity; | Step A: Preparation of Imidazo[l,2-alpha]pyridine-8-carboxylic Acid.2-Aminonicotinic acid (2.0 g, 14.48 mmol) and 2-bromo-l,l-diethoxyethane (2.247 mL, 14.48 mmol) in acetonitrile (10 mL) were heated at 150 0C for 2 h under microwave irradiation. The resulting precipitate was filtered off and washed with acetonitrile and hexane to afford the title compound (2.783 g) as a solid. Exact mass calculated for C8H6N2O2: 162.0. Found: LCMS mlz = 163.1 (M + H)+. 1H NMR (400 MHz, Methanol-^) delta 7.62 (dd, J = 6.82, 7.33 Hz, IH), 8.06 (d, J = 2.27 Hz, IH), 8.36 (d, J = 2.02 Hz, IH), 8.62 (d, J = 7.33 Hz, IH), 9.04 (d, J = 6.82 Hz, IH). Step B: Preparation of 3-Bromoimidazo[l,2-alpha]pyridine-8-carboxylic Acid.Imidazo[l,2-alpha]pyridine-8-carboxylic acid (100 mg, 617 mumol), l-bromopyrrolidine-2,5- dione (110 mg, 617 mumol) and N,N-dimethylformamide (1.5 mL) were stirred at room temperature for 1 h. The resulting precipitate was filtered off and washed with acetonitrile and hexane to afford the title compound as a solid (68 mg). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In acetonitrile; at 150℃; for 2h;microwave irradiation;Product distribution / selectivity; | Example 1.3: Preparation of (4-(2,4-Difluorophenethyl)piperazin-l-yl)(imidazo[l,2- alpha]pyridin-8-yl)methanone (Compound 3).Step A: Preparation of Imidazo[l,2-alpha]pyridine-8-carboxylic Acid.To a mixture of 2-aminonicotinic acid (0.6906 g, 5.00 mmol) in acetonitrile (20 mL) was added bromoacetaldehyde dimethyl acetal (0.591 mL, 5.00 mmol). The resulting slurry was heated at 150 0C under microwave irradiation for 2 h. The resulting precipitate was filtered off and washed with acetonitrile and hexane to afford the title compound (0.924 g) as a grey solid. | |
0.924 g | In acetonitrile; at 150℃; for 2h;Microwave irradiation; | To a mixture of 2-aminonicotinic acid (0.69 g, 5.00 mmol) in CH3CN (20 mL) was added bromoacetaldehyde dimethyl acetal (0.59 mL, 5.00 mmol). The resulting slurry was heated to 150 C under microwave irradiation for 2 h. The resulting precipitate was filtered off and washed with CH3CN and hexane to afford H-imidazo[1,2-alpha]pyridine-8-carboxylic acid (0.924 g) as a grey solid. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With N-Bromosuccinimide; In N,N-dimethyl-formamide; at 20℃; for 1h; | Step B: Preparation of 3-Bromoimidazo[l,2-alpha]pyridine-8-carboxylic Acid.Imidazo[l,2-alpha]pyridine-8-carboxylic acid (100 mg, 617 mumol), l-bromopyrrolidine-2,5- dione (110 mg, 617 mumol) and N,N-dimethylformamide (1.5 mL) were stirred at room temperature for 1 h. The resulting precipitate was filtered off and washed with acetonitrile and hexane to afford the title compound as a solid (68 mg). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With 2,4,6-tripropyl-1,3,5,2,4,6-trioxatriphosphinane-2,4,6-trioxide; triethylamine; In ethyl acetate; N,N-dimethyl-formamide; for 2h;Product distribution / selectivity; | Step E: Preparation of (4-(2,4-Difluorophenethyl)piperazin-l-yl)(imidazo[l,2- alpha]pyridin-8-yl)methanone (Compound 3).To a solution of imidazo[l,2-alpha]pyridine-8-carboxylic acid (36.6 mg, 226 mumol), l-(2,4- difluorophenethyl)piperazine hydrochloride (45.0 mg, 150 mumol) and triethylamine (210 mul, 1504 mumol) in DMF (0.75 mL) was added 1-propylphosphonic acid anhydride solution (50% in ethyl acetate, 183 muL, 0.301 mmol). The mixture was stirred for 2 h, quenched with water and purified by preparative HPLC/MS. The resultant lyophilate was dissolved in DCM, treated with <n="55"/>MP-carbonate resin (-200 mg). The mixture was stirred for 30 min and filtered to remove the resin. The solvent was removed under reduced pressure to afford the title compound as a white solid (33.0 mg). |
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