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CAS No. : | 351410-62-3 | MDL No. : | MFCD04972398 |
Formula : | C7H6FNO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | YAGPZRLCMRMSFP-UHFFFAOYSA-N |
M.W : | 155.13 | Pubchem ID : | 22678323 |
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 |
---|---|---|
42% | With pyridine hydrochloride; at 145℃; for 0.166667h; | Preparation 12 l-Ethyl-5-fluoro-2-oxo-pyridine-3-carbaldehyde (a) 5-Fluoro-2-oxo-pyridine-3-carbaldehyde A flask containing 5-fluoro-2-methoxy-pyridine-3-carbaldeliyde (1.551 g, 10.0 mmol) and pyridine hydrochloride (6.9 g, 60.0 mmol) was heated at 1450C for 10 minutes. The molten mixture was congealed when cooled. Water and EtOAc were added and the pyridine hydrochloride was removed with the water-phase. The water phase was then extracted with EtOAc (3x) and the combined organic phases were dried over MgSO4. Evaporation gave 0.592 g (42 %) of 5-fluoro-2-oxo- pyridine-3-carbaldehyde. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
To a solution of 25 mg (0.063 mmol) l-biphenyl-3-yl~5-[(4-methoxybenzyl)oxy]-2- methylpyridin-4(lH)-one in 1.2 ml of THF was added 94 mu (0.094 mmol) 1 M LiHMDS in THF. After 30 seconds, 9.8 mg (0.063 mmol) <strong>[351410-62-3]5-fluoro-2-methoxynicotinaldehyde</strong> was added. The reaction was quenched with 2 ml of water, extracted with 6 ml of EtOAc, and the organic layer was concentrated in vacuo. The residue was dissolved in 1 ml CH2CI2 and 1 ml TFA was added. The solution was concentrated in vacuo and purified by reverse phase HPLC to yield 1 -biphenyl- 3-yl-2-[2-(5-fluoro-2-methoxypyridin-3-yl)-2-hydroxyethyl]-5-hydroxypyridin-4(lH)-one. NMR delta (pprn)(DMSO-d6): 8.00-7.90 (2 H, m), 7.86 (1 H, s), 7.78 (3 H, d, J = 8.48 Hz), 7.71 (1 H, d, J = 8.95 Hz), 7.52 (3 H, t, J = 7.96 Hz), 7.47-7.39 (2 H, m), 6.79 (1 H, s), 4.73 (1 H, s), 2.94 (2 H, d5 J = 16.33 Hz), 2.73 (1 H, d, J = 10.74 Hz), 2.54 (3 H, s). HRMS (ESI positive) calc (M+H)+ 433.1558 found 433.1562. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium hydroxide; at 20℃; | General procedure: To 3,5-dimethyl-4-(lH-pyrrolo[2,3-b]pyridin-5- yl)isoxazole (P-0246, 0.08 g, 0.35 mmol) in methanol (10 mL) were added 2-chlorobenzaldehyde (0.07 g, 0.5 mmol) and potassium hydroxide (0.3 g, 0.01 mol). The reaction was stirred at room temperature overnight. The reaction was poured into water, extracted with ethyl acetate. The organic layer was washed with brine, and the organic layer was dried over sodium sulfate, concentrated, and purified with silica gel column chromatography eluting with 2% to 20% methanol in methylene chloride to give product (P- 0019, 0.090 g, 72.3%), MS (ESI) [M+H+]+ = 354.1 ; and product (P-0020, 4.4 mg, 4.4%), MS (ESI) [M+H+]+ = 367.8. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
57% | With manganese(IV) oxide; In ethyl acetate; at 20℃; | To (5-fluoro-2-methoxy-pyridin-3-yl)-methanol (36, 8 g, 50.9 mmol) in 300 mL of ethyl acetate, manganese(IV) oxide (39.8 g, 458 mmol) was added and the mixture stirred at room temperature overnight. The reaction mixture was filtered through celite, and the celite bed rinsed with ethyl acetate. The filtrate was concentrated under vacuum, then passed through a plug of silica, eluting with 50% ethyl acetate in heptane to provide the desired compound as a light yellow solid (37, 4.5 g, 29.0 mmol, 57.0% yield). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethylsilane; trifluoroacetic acid; In acetonitrile; at 80℃; for 18h; | To 3-methoxy-5-(5-methyl-1H-pyrrolo[2,3-b]pyridin-3-ylmethyl)-pyridin-2-ylamine (128, 1 equivalent) in 2 mL of acetonitrile, <strong>[351410-62-3]5-fluoro-2-methoxy-pyridine-3-carbaldehyde</strong> (37, 1 equivalent), triethylsilane (5 equivalents) and trifluoroacetic acid (6.9 equivalents) are added. The reaction is heated at 80 C. for 18 hours, then concentrated under vacuum and mixed with aqueous potassium carbonate and extracted with ethyl acetate. The organic layer is washed with water, brine, then dried over magnesium sulfate, filtered and the filtrate concentrated under vacuum. The resulting material is purified by silica gel column chromatography eluting with ethyl acetate and hexane. Appropriate fractions are combined and concentrated under vacuum to provide the desired compound. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
367 mg | With triethylsilane; trifluoroacetic acid; In acetonitrile; at 80℃; for 4h; | To 5-(1-benzenesulfonyl-5-bromo-1H-pyrrolo[2,3-b]pyridin-3-ylmethyl)-6-fluoro-pyridin-2-ylamine (167, 0.342 g, 0.741 mmol) in 10 mL of acetonitrile, <strong>[351410-62-3]5-fluoro-2-methoxy-pyridine-3-carbaldehyde</strong> (37, 0.118 g, 0.763 mmol), triethylsilane (0.529 mL, 3.71 mmol) and trifluoroacetic acid (0.286 mL, 3.71 mmol) were added. The reaction was heated at 80 C. for 4 hours, then concentrated under vacuum and combined with aqueous potassium carbonate and extracted with ethyl acetate. The organic layer was washed with water and brine, then dried over magnesium sulfate, filtered and the filtrate concentrated under vacuum. The resulting material was purified by silica gel column chromatography eluting with ethyl acetate and hexane. Appropriate fractions were combined and concentrated under vacuum to provide the desired compound as an off-white solid (168, 367 mg). MS (ESI) [M-H+]-=599.6 and 601.6. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethylsilane; trifluoroacetic acid; at 80℃; | To 5-(5-bromo-1H-pyrrolo[2,3-b]pyridin-3-ylmethyl)-6-fluoro-pyridin-2-ylamine (173, 1 equivalent) and <strong>[351410-62-3]5-fluoro-2-methoxy-pyridine-3-carbaldehyde</strong> (37, 1 equivalent), triethylsilane (4 equivalents) and trifluoroacetic acid (4 equivalents) are added. The reaction is stirred at 80 C. for several hours, then concentrated under vacuum. The resulting material is taken up in ethyl acetate and extracted with addition of aqueous potassium carbonate. The organic layer is concentrated under vacuum, then triturated with dichloromethane to provide the desired compound. |
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