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CAS No. : | 128495-46-5 | MDL No. : | MFCD00143320 |
Formula : | C8H7FO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | NALVGTOMKSKFFV-UHFFFAOYSA-N |
M.W : | 154.14 | Pubchem ID : | 2737358 |
Synonyms : |
|
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 |
---|---|---|
85% | With manganese(IV) oxide; In dichloromethane; for 16h;Heating / reflux; | (4-FLUORO-3-METHOXYPHENYL) METHANOL (5. 00G, 0. 03mol) and manganese dioxide (33.4g, 0. 38MOL) were stirred in DICHLOROMETHANE (100ml) under an atmosphere of nitrogen, at gentle reflux for 16 hours. The cooled reaction mixture was then filtered through arbacel and concentrated in vacuo to give the title compound as a white solid (4.18g, 0. 027MOL, 85%). 1H NMR (CDCI3, 400MHZ) 8 : 3.96 (s, 3H), 7.23 (d, 1H), 7.43 (m, 1 H), 7.50 (d, 1 H) 9.91 (s, 1H). Mpt: 61-63C. Analysis found C, 62.18 ; H, 4.54%. C8H7FO2 requires C, 62.34 ; H, 4.58%. |
85% | With manganese(IV) oxide; In dichloromethane; for 16h;Heating / reflux; | (4-Fluoro-3-methoxyphenyl) methanol (5.0Og, 0.03mol) and manganese dioxide (33.4g, 0.38mol) were stirred in dichloromethane (100ml) under an atmosphere of nitrogen, at gentle reflux for 16 hours. The ? cooled reaction mixture was then filtered through arbacel and concentrated in vacuo to give the title compound as a white solid (4.18g, 0.027mol, 85%). 1H NMR (CDCI3, 400MHz) δ: 3.96 (s, 3H), 7.23 (d, 1 H), 7.43 (m, 1 H), 7.50 (d, 1 H) 9.91 (s, 1 H). Mpt: 61-630C. Analysis found C, 62.18; H, 4.54%. C8H7FO2 requires C, 62.34; H, 4.58%. |
81% | With chromium trioxide pyridine; In dichloromethane; at 20℃; for 0.5h; | To a solution of (4-fluoro-3-methoxyphenyl) methanol (1.56 g, 10 mmol) in dichloromethane (40 mL) was added chromium trioxide pyridine (4.31 g, 20 mmol). The mixture was stirred at room temperature for 30 min and filtered. The filtrate was poured onto a short silica gel column, and eluted with dichloromethane. The resulting solution was concentrated under vacuum to afford the title compound (1.25 g, 81 %). 1H NMR (CDCl3): δ 9.92 (1H, s), 7.52 (1H, dd, J = 2.0 Hz, 8.4 Hz), 7.47-7.43 (1H, m), 7.26-7.22 (1H, m), 3.96 (3H, s). |
81% | With pyridine; chromium(VI) oxide; In dichloromethane; at 20℃; for 0.5h; | To a solution of (4-fluoro-3-methoxyphenyl) methanol (1.56 g, 10 mmol) in dichloromethane (40 mL) was added chromium trioxide pyridine (4.31 g, 20 mmol). The mixture was stirred at room temperature for 30 min and filtered. The filtrate was poured onto a short silica gel column, and eluted with dichloromethane. The resulting solution was concentrated under vacuum to afford the title compound (1.25 g, 81 %). 1H NMR (CDCl3): δ9.92 (1H, s), 7.52 (1H, dd, J=2.0 Hz, 8.4 Hz), 7.47-7.43 (1H, m), 7.26-7.22 (1H, m), 3.96 (3H, s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With sodium hydroxide; sodium tetrahydroborate; In methanol; water; for 1h; | Preparation 44; To a solution of 4-fluoro-3-methoxybenzaldehyde (5 g) in methanol (25 ml) was added dropwise sodium borohydride (368 mg) in 0.1N sodium hydroxide aqueous solution (5 ml) in water bath and the whole was stirred for 1 hour. After the mixture was evaporated under reduced pressure, ethyl acetate and water were added thereto. The organic layer was separated and the water layer was further extracted with ethyl acetate. The combined organic layer was dried over magnesium sulfate and concentrated in vacuo to give 4-fluoro-3-methoxybenzyl-alcohol (5.22 g) as an oil. IR (Neat): 1610, 1516, 1462, 1417, 1315, 1277, 1149, 1115, 1032 cm-1 NMR (CDCl3, δ): 1.75 (1H, br s), 3.90 (3H, s), 4.64 (2H, s), 6.70-7.20 (3H, m) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium carbonate; In N,N-dimethyl-formamide; at 80℃; | 1H-imidazole (42.0 mg) and potassium carbonate (180 mg) were added to a solution of 4-fluoro-3-methoxybenzaldehyde (100 mg) in DMF (2.0 mL), and the reaction solution was stirred at 80C overnight. Water and ethyl acetate were added to the reaction solution, and the organic layer was separated. The resulting organic layer was washed with brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system -> ethyl acetate-methanol system) to obtain 36.2 mg of the title compound. The property values of the compound are as follows. 1H-NMR (CDCl3) delta (ppm): 3.98 (s, 3H), 7.21 (s, 1H), 7.30 (s, 1H), 7.48 (d, J = 7.6 Hz, 1H), 7.56-7.60 (m, 2H), 7.92 (s, 1H), 10.0 (s, 1H). | |
With potassium carbonate; In N,N-dimethyl-formamide; at 130℃; | l-(4-Ethynyl-2-methoxyphenyl)-l//-imidazole.A mixture of 4-fiuoro-3-methoxybenzaldehyde (1.0 g, 6.5 mmol) in 20 mL of DMF was treated with 4-methylimidazole (1.0 g, 15 mmol) and warmed to 130 C. Stirred overnight. Diluted with EtOAc, washed with sat'd NaHCO3, dried (Na2SO4), concentrated. Dissolved in 20 mL of MeOH, treated with K2CO3 (2.0 g, 14 mmol) and dimethyl (l-diazo-2-oxopropyl)phosphonate (1.5 g, 7.8 mmol) and stirred overnight. Diluted with DCM and washed with water. Dried (Na2SO4), cone. Chromatography on silica (0-20% MeOH/DCM) gave the desired alkyne:1H NMR (600 MHz, CDCl3) delta7.79 (s, 1 H), 7.18 (t, J= 1.2 Hz, 1 H), 7.16 (d, J= 1.8 Hz, 1 H), 7.15 (m, 2 H), 7.13 (d, J= 1.5 Hz, 1 H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
35% | Intermediate 104-fluoro-3-(methyloxy)phenolTo a solution of 4-fluoro-3-(methyloxy)benzaldehide (1.54 g, 10 mmol) in DCM (30 mL) metachloroperbenzoic acid (2.59 g, 15 mmol) was added portionwise and the reaction mixture was stirred for 3 hours at room temperature. A second portion of m-CPBA (2.59 g, 15 mmol) wasadded and the reaction mixture was stirred for further 18 hrs. The mixture was diluted with DCM (100 mL), washed with an aqueous saturated solution of Na25203 (2x100 mL) and then with an aqueous saturated solution of NaHCO3(50 mL), dried over Na2SO4 and concentrated in vacuo to yield a yellow gum, which was re-dissolved in MeOH (20 mL) and Triethylamine (0.1 ml) was added. The reaction mixture was stirred for 18 hrs at room temperature and concentrated in vacuo. The residue was re-dissolved in Et20 (100 mL) and extracted with an aqueous iN solution of NaOH (50 mL). The aqueous layer was acidified with aqueous 2N HCIto pH=1 and extracted with Et20 (2x50 mL). The combined organic layers were dried overNa2SO4 and concentrated in vacuo to afford the title compound (830 mg, yield: 35percent).1HNMR (400 MHz, CDCI3): 6 ppm 6.81-6.85 (1H, t), 6.40-6.43 (1H, m), 6.21-6.24 (1H, m), 4.61(1H, s), 3.76 (3H, s). |
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