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CAS No. : | 81719-53-1 | MDL No. : | MFCD03230005 |
Formula : | C6H3Cl2NO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | JYKZCYLZWZCQFP-UHFFFAOYSA-N |
M.W : | 192.00 | Pubchem ID : | 219989 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
3,5-Dichloropyridine-2-carboxylic Acid (CAS: 81719-53-1) has been used in the preparation of Vadadustat (CAS: 1000025-07-9). Vadadustat is employed for the treatment of symptomatic anemia related to chronic kidney disease in adults undergoing chronic maintenance dialysis.
* 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 |
---|---|---|
100% | With oxalyl dichloride;N,N-dimethyl-formamide; In dichloromethane; at 0 - 20℃; for 2h; | 3,5-dichloro-2-(chloromethyl)pyridine; [00376] To a 0 C solution of 5-chloropicolinic acid (5.00 g, 26.0 mmol) and N,N- dimethylformamide (1 drop) in dichloromethane (20 mL) was added oxalyl chloride (3.28 g, 26.0 mmol) dropwise, after which the reaction mixture was allowed to warm up to room temperature and stirred at that temperature for two hours. The reaction was then cooled again to 0 C, after which methanol (10 mL) was added dropwise to the reaction mixture, and the reaction was allowed to stir at room temperature for one hour where it was shown as complete by LCMS analysis. The reaction mixture was washed with saturated sodium bicarbonate solution, dried (magnesium sulfate), filtered and concentrated to afford methyl 3,5-dichloropyridine-2-carboxylate (5.36 g, 26.0 mmol, 100% yield ) as a white solid.[00377] To a 0 C solution of methyl 3,5-dichloropyridine-2-carboxylate (5.00 g, 24.3 mmol) in methanol (40 mL) was added sodium borohydride (1.80 g, 48.5 mmol), after which the reaction was warmed to room temperature and stirred at that temperature for two hours. The reaction mixture was then quenched by the addition of water (5 mL), concentrated to a residue, reconstituted in water (60 mL), extracted with ethyl acetate (2 x 60 mL), dried (magnesium sulfate), filtered and concentrated to afford (3,5-dichloropyridin-2-yl)methanol (2.90 g, 16.3 mmol, 67% yield ) as a viscous oil. This material was used in the subsequent step without any purification.[00378] To a 0 C solution of (3,5-dichloropyridin-2-yl)methanol (2.90 g, 16.3 mmol) in dichloromethane (50 mL) was added thionyl chloride (2.31 g, 19.6 mmol) dropwise, after which the reaction mixture was allowed to warm up to room temperature and stirred at that temperature for two hours. The reaction mixture was washed by the addition of saturated sodium bicarbonate solution (1 x 40 mL) and the organic layer was separated, dried (sodium sulfate), filtered and concentrated to a residue. Purification was achieved by silica gel chromatography using 9% ethyl acetate in hexanes to afford 3,5-dichloro-2- (chloromethyl)pyridine (2.40 g, 12.2 mmol, 75% yield) as an off-white solid. NMR (300 MHz, CDC13) delta (ppm): 8.36 (s, 1H), 7.56 (s, 1H), 4.66 (s, 2H). |
100% | With oxalyl dichloride; N,N-dimethyl-formamide; In dichloromethane; toluene; at 0 - 20℃; for 2.5h; | 3,5-Dichloropicolinic acid (61.5 mg, 320 muiotaetaomicron) was suspended in dichloromethane (5 mL), the suspension was cooled to 0-5C (ice bath) and oxalyl chloride (56.9 mg, 39.3 mu, 448 muiotaetaomicron) as well as dimethylformamide (0.308 M in toluene, 48 mu, 15 muiotaetaomicron) were added. The mixture was stirred for 2.5 h at room temperature. Then, it was concentrated in vacuo (40C, 5 mbar) and dried azeotropically by two cycles of addition of toluene (3 mL) followed by concentration in vacuo to afford 3,5-dichloropicolinoyl chloride as yellow oil (67 mg, quant.). After that, tert-butyl ((3aS,4R,8R)-4-(5-amino-2-fluorophenyl)-4,7,7-trimethyl-8-oxido-3,3a,4,7- tetrahydro-2H-isothiazolo[l,5-a][l,4]thiazin-6-yl)carbamate (Int-16ABp, 80 mg, 188 muetaiotaomicron) was dissolved in dichloromethane (5 mL), the solution cooled to 10C and N,N- diisopropylethylamine (41.4 mg, 56 mu, 320 mumol) was added, followed by a solution of 3,5- dichloropicolinoyl chloride (vide supra, 54 mg, 256 muiotaetaomicron) in dichloromethane (4 mL). The reaction mixture was stirred for 15 min at 10C. Then, methanol (2 mL) was added, the mixture was stirred for 5 min at room temperature and concentrated in vacuo. The crude was purified by column chromatography (silica gel, 12 g, eluting with ethyl acetate / n-heptane, gradient 30:70 to 100:0) to yield, after drying in vacuo (40C, 5 mbar), the title compound as a light brown solid (103 mg, 92%). HPLC (method LCMS_fglm) tR = 1.34 min. MS (ES+) m/z 598.4 [M+H]. |
100% | With thionyl chloride; In N,N-dimethyl-formamide; at 60℃; for 2h; | N,N-Dimethylfonnamide (0.05 mL, 0.60 mmol) was added to <strong>[81719-53-1]3,5-dichloropicolinic acid</strong> (15 g, 78 mmol). The mixture was treated with thionyl chloride (45 mL, 620 mmol) and heated at 60 C for 2 hours. The solution was cooled to ambient temperature and concentrated in vacuo. Toluene (50 mL) was added and the mixture was concentrated and dried in vacuo to afford methyl 3,5-dichioropicolinic acid chloride as a light tan solid (17 g, 100% yield).1H NMR (500 MHz, chloroform-d) oe (ppm) 8.64 (d, 1 H), 7.93 (d, 1 H). |
With thionyl chloride;N,N-dimethyl-formamide; for 0.25h;Heating / reflux; | Example 54(a) 3,5-Dichloro-2-(piperidin-l-ylcarbonyl)pyridine; 3,5-Dichloro-2-pyridine carboxylic acid (1.25 g, 6.5 mmol) was suspended in thionyl chloride (10 ml). DMF (2 drops) was added and the mixture was refluxed for 15 minutes under an atmosphere of nitrogen. The solvent was evaporated. Toluene was added and the solvent was evaporated to give a solid. The solid was dissolved in DCM (8 ml) and the mixture was cooled to 0 C. Piperidine (0.64 ml, 6.5 mmol) was added dropwise followed by triethylamine (0.91 ml, 6.5 mmol). The cooling bath was removed. The mixture was <n="76"/>stirred under nitrogen atmosphere until RT was reached and then for an additional 15 minutes. The mixture was washed with aqueous sodium bicarbonate and the organic phase was dried (MgSO4), filtered and concentrated. The residue was purified by column chromatography eluting with gradients of heptane and ethyl acetate to give the title compound (1.28 g, 76%).1H NMR (400 MHz, CDCl3) delta ppm 8.46 (d, 1 H) 7.77 (d, 1 H) 3.74 (m., 2 H) 3.11 - 3.16 (m, 2 H) 1.64 - 1.71 (m, 4 H) 1.55 (m, 2 H) MS (ESI) m/z 259; 261 (M+l). | |
With thionyl chloride; N,N-dimethyl-formamide; In toluene; for 2h;Reflux; | A mixture of 3,5-dichloro-pyndme-2-carboxylic acid (5 76 g, 30 mmol) and thionyl chloride (44 mL, 60mmol) in 50 mL of anhydrous toluene and 0 5 mL of anhydrous DMF was refluxed for 2 h The solvent was removed under reduced pressure to give a mobile oil residue which was azeoptoped with toluene (2OmL) The residue was dissolved in 20 mL of anhydrous THF and this solution was added dropwise to a solution of ethyl 3-(dimethylamino)acrylate (47g, 33 mmol) and triethylamine (3 64 g, 36 mmol) in 20 mL of anhydrous THF under nitrogen, and the mixture was heated under reflux for 7 hours The reaction mixture was allowed to cool to room temperature and concentrated under reduced pressure Water (10OmL) and ethyl acetate (10OmL) was added to allow partitioning The organic layer was washed successively with saturated aqueous sodium bicarbonate(x2), water, brine, dried over sodium sulfate and was concentrated under reduced pressure The crude product was purified by ISCO (hexane/EtOAc, 0-40%, 30 mm, 100%, 20 mm) to give 5 9 g (62%) of pure product as yellow oil | |
110 mg | With oxalyl dichloride; N,N-dimethyl-formamide; In dichloromethane; toluene; at 0 - 20℃; for 1.5h; | 3,5-Dichloropicolinic acid (200 mg, 1.04 mmol) was suspended in dichloromethane (4 mL), the suspension was cooled to 0-5C (ice bath) and oxalyl chloride (363 mg, 250 mu, 2.86 mmol,) as well as a drop of a mixture of dimethylformamide and toluene (1:3, v/v) were added. The mixture was stirred for 1.5 h at room temperature. Then, it was concentrated in vacuo at 40C, the residue was treated with n-heptane (4 mL) and again concentrated and dried in vacuo (40C, 5 mbar) to afford 3,5-dichloropicolinoyl chloride as yellow solid (110 mg). After that, tert-butyl ((4aR,5R,9R)-5-(6-amino-3-fluoropyridin-2-yl)-5,8,8-trimethyl-9-oxido-2,3,4,4a,5,8- hexahydro-[l,4]thiazino[2,l-f] [l,2]thiazin-7-yl)carbamate (Int-17AA, 100 mg, 228 mupiiotaomicron) was dissolved in dichloromethane (4 mL), the solution cooled to 0-5C (ice bath) and N,N- diisopropylethylamine (75.5 mg, 100 mu, 584 muiotaetaomicron) was added, followed by a solution of 3,5- dichloropicolinoyl chloride (vide supra, 60 mg, 285 muiotaetaomicron) in dichloromethane (1.2 mL).The reaction mixture was stirred at 0-5C for 1.5 h. Then, ethanol (100 mu) was added, the mixture was stirred for 45 min at room temperature, poured onto a saturated aqueous solution of sodium hydrogencarbonate (15 mL) and extracted with dichloromethane (1 x 30 mL, 2 x 20 mL). The combined extracts were dried (sodium sulfate) and concentrated in vacuo. The crude was purified by column chromatography (silica gel, 50 g, eluting with ethyl acetate / n-heptane, gradient 60:40 to 80:20) to yield, after drying in vacuo (50C, 5 mbar), the title compound as a light yellow foam (140 mg, 99% yield). HPLC (method LCMS_gradient) tR = 3.2 min. XH NMR (CDC13, 400 MHz): delta 1.48 (s, 9 H), 1.79 (s, 3 H), 1.81-2.02 (m, 3 H), 1.85 (s, 3 H), 1.95 (s, 3 H), 2.40 (dddd, J = 3.8, 12.6, 12.6, 12.6 Hz, 1 H), 3.36-3.43 (m, 1 H), 3.58-3.66 (m, 1 H), 4.08 (dd, J = 3.2, 12.4 Hz, 1 H), 7.57 (dd, .7 = 8.9, 10.7 Hz, 1 H), 7.95 (d, 7 = 2.1 Hz, 1 H), 8.44 (dd, / = 3.1, 9.0 Hz, 1 H), 8.57 (d, J = 1.9 Hz, 1 H), 10.16 (br s, 1 H, exch), 11.23 (br s, 1 H, exch). MS (ES+) m/z 613.3, 615.3 & 617.3 [M+H, 2 CI] . |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethylamine; In dichloromethane; at 0 - 20℃; for 0.25h; | Example 54(a) 3,5-Dichloro-2-(piperidin-l-ylcarbonyl)pyridine; 3,5-Dichloro-2-pyridine carboxylic acid (1.25 g, 6.5 mmol) was suspended in thionyl chloride (10 ml). DMF (2 drops) was added and the mixture was refluxed for 15 minutes under an atmosphere of nitrogen. The solvent was evaporated. Toluene was added and the solvent was evaporated to give a solid. The solid was dissolved in DCM (8 ml) and the mixture was cooled to 0 C. Piperidine (0.64 ml, 6.5 mmol) was added dropwise followed by triethylamine (0.91 ml, 6.5 mmol). The cooling bath was removed. The mixture was <n="76"/>stirred under nitrogen atmosphere until RT was reached and then for an additional 15 minutes. The mixture was washed with aqueous sodium bicarbonate and the organic phase was dried (MgSO4), filtered and concentrated. The residue was purified by column chromatography eluting with gradients of heptane and ethyl acetate to give the title compound (1.28 g, 76%).1H NMR (400 MHz, CDCl3) delta ppm 8.46 (d, 1 H) 7.77 (d, 1 H) 3.74 (m., 2 H) 3.11 - 3.16 (m, 2 H) 1.64 - 1.71 (m, 4 H) 1.55 (m, 2 H) MS (ESI) m/z 259; 261 (M+l). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85% | With sulfuric acid; water; at 115℃; | 3,5-Dichloro-pyridine-2-carbonitrile (10 g, 57 8 mmol) was dissolved in 100 mL of 95% concentrated sulfuric acid and this mixture was heated to 115 C overnight The reaction mixture was then cooled, poured over ice with strong stirring The resulting solid was filtered, washed with water and dried at 40 C under reduced pressure to give 94g (85%) of pure product as a white solid |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Ninth step To a stirred under ice-cooling solution of <strong>[81719-53-1]3,5-dichloropyridine-2-carboxylic acid</strong> in N,N-dimethylformamide (0.5 ml), 2-(1H-7-azabenzotriazol-1-yl)-1,1,3,3-tetramethyluronium hexafluorophosphate (0.05 mg) and triethylamine (0.01 mg) were added. After stirred for 10 minutes, a solution of the compound (116) (0.05 g) in N,N-dimethylformamide (2 ml) was added, and the mixture was stirred at room temperature for 2.5 hours. Water was added, the mixture was extracted with ethyl acetate, and the organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was subjected to silica gel column chromatography to afford the compound (117) (0.05 g). 1H-NMR (CDCl3) delta: 3.89 (1H, d, J = 11.7 Hz), 3.99 (1H, d, J = 11.7 Hz), 4.26 (1H, t, J = 6.8 Hz), 4.47 (3H, d, J = 6.8 Hz), 6.96 (1H, dd, J = 8.9, 7.2 Hz), 7.10-7.14 (2H, m), 7.28-7.42 (9H, m), 7.60 (2H, d, J = 7.3 Hz), 7.74-7.76 (2H, m), 7.90 (1H, d, J = 2.0 Hz), 8.46 (1H, d, J = 2.0 Hz), 9.77 (1H, s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; In dichloromethane; at 22℃; for 16h; | Synthesis of the amides H and IGeneral ProcedureTo a solution of the aniline G (0.32 mmol) in dry dichloromethane (5 ml) was added subsequently EDCI (0.35 mmol), the carboxylic acid (0.35 mmol) and stirring was continued at 22 C. for 16 h. The mixture was purified on prep. RP-18 HPLC using a gradient of acetonitrile and water (containing 0.1% of triethylamine) to give the t-butyloxycarbonyl protected intermediate H.A solution of t-butyloxycarbonyl protected intermediate H (0.27 mmol) in 4.0 ml dry dichloromethane was added CF3COOH (1 ml) and stirring was continued at 22 C. for 90 min. The mixture was evaporated, the residue was dissolved in DMSO and purified by prep. RP-18 HPLC using a gradient of acetonitrile and water (containing 0.1% of triethylamine) to give the pure amide I in yields of 10-70%.; Example 13,5-Dichloro-pyridine-2-carboxylic acid [3-((S)-2-amino-4-methyl-5,6-dihydro-4H-[1,3]oxazin-4-yl)-4-fluoro-phenyl]-amideThe coupling of [(S)-4-(5-amino-2-fluoro-phenyl)-4-methyl-5,6-dihydro-4H-[1,3]oxazin-2-yl]-carbamic acid tert-butyl ester from experiment F1 (R3=Me) and <strong>[81719-53-1]3,5-dichloro-pyridine-2-carboxylic acid</strong> followed by deprotection using procedure H yielded the title compound.MS (ESI): m/z=398.1 [M+H]+. | |
With 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; In dichloromethane; at 22℃; for 16h; | To a solution of the aniline G (0.32 mmol) in dry dichloromethane (5 ml) was added subsequently EDCI (0.35 mmol), the carboxylic acid acid (0.35 mmol) and stirring was continued at 22 C for 16 h. The mixture was purified on prep. RP-18 HPLC using a gradient of acetonitrile and water (containing 0.1 % of triethylamine) to give the t-butyloxycarbonyl protected intermediate H.A solution of t-butyloxycarbonyl protected intermediate H (0.27 mmol) in 4.0 ml dry dichloromethane was added CF3COOH (1 ml) and stirring was continued at 22 C for 90 min. The mixture was evaporated, the residue was dissolved in DMSO and purified by prep. RP-18 HPLC using a gradient of acetonitrile and water (containing 0.1 % of triethylamine) to give the pure amide I in yields of 10-70%.The coupling of [(S)-4-(5-amino-2-fluoro-phenyl)-4-methyl-5,6-dihydro-4H-[l,3]oxazin-2- yl]-carbamic acid tert-butyl ester from experiment Fl (R3= Me) and 3,5-dichloro-pyridine-2- carboxylic acid followed by deprotection using procedure Eta yielded the title compound. MS (ESI): m/z = 398.1 [M+H]+. |
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