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CAS No. : | 455-93-6 | MDL No. : | MFCD00061095 |
Formula : | C7H6FNO3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | XGMVTXUXZUPGGY-UHFFFAOYSA-N |
M.W : | 171.13 | Pubchem ID : | 223104 |
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 |
---|---|---|
In ethanol; water; acetic anhydride; | 2-Fluoro-4-nitroanisole (IX) To a cold (-2), stirred solution of 285 g. (2.26 mol) of 2-fluoroanisole in 1.1 L of acetic anhydride was added, dropwise, 114 mL of fuming nitric acid (sp. gr. 1.59) at such a rate that the reaction temperature remained between -2 and 0. The reaction mixture was stirred for 5 hours at this temperature then poured into 4.0 L of water. The suspension was stirred for 1.5 hours, stored for 15 hours, then extracted with methylene chloride (2*1.0 L). The combined extracts were washed with water (2*500 mL), dried over anhydrous magnesium sulfate, then concentrated in vacuo (475 g.). Crystallization from ethanol gave 147.4 g. (38%) of material suitable for further transformation. Additional material (34.5 g.) was obtained from three scouting runs. Analytically pure product (5.2 g.; 63.4% recovery) was obtained by recrystallizing 8.2 g of the material from 200 mL of ethanol; mp, 105-106 (Literature, R. C. Elderfield et al., J. Am. Chem. Soc., 68, 1584 (1946)). Anal. Calcd for C7 H6 FNO3 (percent): C, 49.13; H, 3.53; F, 11.10; N, 8.19. Found: C, 49.07; H, 3.52; F, 11.02; N, 8.19. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98% | With palladium on activated charcoal; In ethyl acetate; at 20℃; for 1h; | 3-Fluoro-4-methoxy-nitrobenzene (0.5 g, 2.9 mmol) was dissolved in ethyl acetate (10 mL) was added palladium on carbon (50 mg), stirred at room temperature for 1 hour. The reaction mixture was filtered, the filtrate was concentrated to give the title compound 3-fluoro-4-methoxyaniline (7B), an off-white solid (0.4 g, 98% yield). |
91% | With hydrogen;palladium 10% on activated carbon; In ethanol; at 20℃; under 2068.65 Torr; for 4h; | To a mixture of 10% Pd/C (1.5 grams) in ethanol (150 mL) taken in a Parr hydrogenation flask was added a solution of <strong>[455-93-6]2-fluoro-4-nitroanisole</strong> (7) (9.09 grams, 53 mmol) in ethanol (150 mL) slowly. The mixture was then stirred under hydrogen atmosphere (40 psi) for 4 hours at room temperature. After completion of the reaction the mixture was filtered through Celite and the residue was washed thoroughly using ethanol (20 mL). The filtrates and washings were collected, combined and evaporated to dryness. The solid obtained was stirred in hexane (50 mL) for 1 hour and filtered to give the desired product 3-fluoro-4-methoxyaniline (8) (6.75 grams). |
78% | With zinc; In water; at 20℃; for 0.0833333h;Inert atmosphere; | General procedure: Under an argon atmosphere, a nitro group-containing compound (0.237 mmol) was weighed into a 5 mL microwave vial containing a magnetic stir bar and a Teflon-lined septum. Subsequently zinc dust (155 mg, 2.37 mmol), ammonium chloride (25 mg, 0.475 mmol) and the aqueous oligosaccharide solution (2 wt % HPMC, 40-60 cps, in degassed Millipore water) were added and the reaction mixture was vigorously stirred at the indicated temperature for the indicated time. The reaction mixture was diluted with ethyl acetate, the solids were filtered and the aqueous phase was extracted 3x with ethyl acetate. The combined organic extracts were dried with magnesium sulfate, filtered and concentrated in vacuo. The crude product was purified by flash chromatography on silica gel.; Following the general procedure using <strong>[455-93-6]2-fluoro-4-nitroanisole</strong> (171 mg, 1.00 mmol), zinc (327 mg, 5.00 mmol), ammonium chloride (64 mg, 1.20 mmol) and 2 ml of aqueous oligosaccharide solution (2 wt % HPMC, 40-60 cps, in degassed Millipore water), the reaction was allowed to stir for 5 min at room temperature. After column chromatography (0-100 % ethyl acetate - dichloromethane), the product was obtained (110 mg, 78 %).ESI-MS: m/z (%): 142.10 (100, [M+H]+).1H NMR (600MHz, d6-OMSO): delta [ppm] : 6.856.31 - 6.28 (m, 1H), 4.91 (sbr, 2H), 3.68 (s, 3H). |
palladium-carbon; In 1,4-dioxane; | [I] 2 g of 5% palladium carbon was added to a solution prepared by dissolving 10 g of <strong>[455-93-6]4-nitro-2-fluoroanisol</strong> in 150 ml of 1,4-dioxane, and the mixture was subjected to catalytic reduction under a hydrogen gas pressure of 4 kg/cm2 at room temperature for 30 minutes. After the completion of the reaction, palladium carbon was removed by filtration, and the solvent was distilled off under reduced pressure to obtain 8.6 g of 4-amino-2-fluoroanisol. |
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