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CAS No. : | 402-69-7 | MDL No. : | MFCD02181193 |
Formula : | C6H4FNO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | DIEMCUFYSOEIDU-UHFFFAOYSA-N |
M.W : | 141.10 | Pubchem ID : | 226027 |
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: |
* 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 |
---|---|---|
53% | With potassium permanganate; In water; for 3h;Heating / reflux; | To [A] solution of 2-fluoro-6-methyl-pyridine (2.5g, 22.5 [MMOL)] in water (170 ml) was added portionwise [KMN04] (2g, 12.65 mmol) and the mixture was heated to reflux. Then [KMN04] (8g, 50.63 [MMOL)] was added portionwise and the mixture was heated under reflux for 3 hours. On cooling, the precipitate was filtered and the filtrate was acidified with a solution of HCI and then concentrated under reduced pressure. The residue was triturated with hot EtOH, the solid was filtered and the filtrate was concentrated to dryness under reduced pressure. The title compound was obtained as a white solid (1.7g, 53percent); m. p. [137°C.] |
53% | With potassium permanganate; In water; for 3h;Heating / reflux; | To a solution of 2-fluoro-6-methyl-pyridine (2.5g, 22.5 [MMOL)] in water (170 ml) was added portion-wise [KMN04] (2g, 12.65 [MMOL)] and the mixture was heated to reflux. [KMN04] [(8G,] 50.63 [MMOL)] was added portion-wise and the mixture was heated under reflux for 3 hours and then cooled. The precipitate was filtered and the filtrate was acidified with a solution of HCI and then concentrated under reduced pressure. The residue was triturated with hot [ETOH,] the solid filtered and the filtrate was concentrated to dryness under reduced pressure. The title compound was obtained as a white solid (1.7g, 53percent); m. p. [137°C.] |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
31% | B. 4-Chloro-2-(difluoromethyl)-1 -[5-(6-fluoro-2-pyridinyl)-1 ,3,4- oxadiazol-2-yl]methyl}-1H-indole-5-carbonitrile; <n="96"/>To a solution of beta-fluoro^-pyridinecarboxylic acid (0.006 g, 0.043 mmol) in MeCN (2 ml_), under N2, was added EDCI (0.0085 g, 0.044 mmol). After 5 min, 2- [4-chloro-5-cyano-2-(difluoromethyl)-1/-/-indol-1-yl]acetohydrazide (0.012 g, 0.040 mmol) was added. After 1 h, additional beta-fluoro^-pyridinecarboxylic acid (0.003 g, 0.02 mmol) and EDCI (0.0077 g, 0.040 mmol) were added. After another 15 min, additional <strong>[402-69-7]6-fluoro-2-pyridinecarboxylic acid</strong> (0.0014 g, 0.01 mmol) and EDCI (0.0046 g, 0.02 mmol) were added. After another 10 min, TsCI (0.009 g, 0.048 mmol) and P-BEMP (loading 2.2 mmol/g, 0.073 g, 0.16 mmol) were added and the mixture was heated at 12O0C for 20 min. Upon cooling, additional TsCI (0.0046 g, 0.024 mmol) and P-BEMP (0.037 g, 0.08 mmol) were added and the mixture was heated at 12O0C for another 20 min. Upon cooling, the resin was filtered off, washed with EtOAc and the filtrate was concentrated in vacuo. The residue was purified by flash chromatography (0-50percent EtOAc-hexanes gradient) and the product was crystallized from CH2CI2-hexanes to give the title compound as a white solid (0.005 g, 31 percent yield): MS (ES) m/z 404 (M+1 ). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium permanganate; at 100℃; for 4h;Heating / reflux; | Add potassium permanganate (12.8 g, 81.0 mmol) to a solution of 2-fluoro-5-methylpyridine (3.0 g, 27.0 mmol) in water (135 ml). Heat the reaction to 100 C for 4hours. While the reaction is hot, filter through Celite Rinse the filter cake with hot water (2 x 50ml) and concentrate the combined aqueous solutions in vacuo to a volume of 50 ml. Acidify with concentrated HCl and concentrate to dryness in vacuo to provide the title compound as a white solid which is used directly in the next step. MS APCI+ m/e 142 (M+1) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With thionyl chloride; for 3h;Heating / reflux; | Intermediate 20 (1g, 7.09 [MMOL)] was added portionwise to thionyl chloride (3 ml) and the mixture was heated under reflux for 3 hours and then concentrated under reduced pressure. Isopropanol (3 ml) was added to the residue and the mixture was stirred at room temperature for 5 minutes and then concentrated under reduced pressure. The residue was treated with a saturated solution of NaHCO3, extracted with ethyl acetate, the organic phase was dried over [NA2SO4] and concentrated under reduced pressure. The title compound was obtained as an cream oil (1.2g, 93percent); [[APCI] MS] m/z: 184 (MH+). | |
With thionyl chloride; for 5h;Reflux; | 2-fluoro-pyridine-6-carboxylic acid in thionyl chloride (2ml) (86mg, 0.448mmol) was heated under reflux for 5 hours stirred suspension of. Then excess reagent was removed under reduced pressure to give a crude solid. The crude solid, 4- (6-methyl-imidazo [1,2-a] pyridin-2-yl) aniline (100 mg, 0.448 mmol) and dry THF (20 ml) and diisopropylethylamine (94mul, 0.539mmol) in the amide prepared as described in the section amide coupling using, work-up and flash chromatography: the (2 1 EtOAc / hexanes) after to give the title compound 85 mg, 55percent) of a colorless solid . |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With dmap; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; In dichloromethane; at 20℃; | EDCI (80 mg) and DMAP (20 mg) are added to a stirred solution of (4,6-diethoxy- PYRIDAZIN-3-YLMETHYL)-3-METHYL-BYTYL)-AMINE (93.5 mg) and fluoropyridinyl acid (59 mg) in DCM (10ML). The mixture is stirred at room temperature overnight. DCM (10 ml) is added to dilute the mixture. The mixture is washed with water (5 mL), dried (NA2S04), and evaporated. Preparative TLC purification of the residue (2: 1 of hexane: ethyl acetate) provides the title product (Compound 2). HL NMR 6 (CDCI3) 7.80-7. 92 (M, 1H), 7.60-7. 68 (M, 1H), 6.95-7. 02 (M, 1H), 6.22 (s, 2H), 4.98 (s, 2H), 4.56 (q, 2H, J = 7.2 Hz), 4.12. |
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