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CAS No. : | 157701-72-9 | MDL No. : | MFCD00968941 |
Formula : | C7H4FNO3 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | ZFCMKFOFVGHQNE-UHFFFAOYSA-N |
M.W : | 169.11 | Pubchem ID : | 4562919 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H332-H335 | Packing Group: | |
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 |
---|---|---|
30% | With manganese(IV) oxide; In dichloromethane; at 20℃; | Add borane-tetrahydrofuran complex (16.21 [ML,] [1] M) to a mixture of 2-fluoro-4- nitro-benzoic acid (1.2 g) and tetrahydrofuran (10 [ML)] at [0C.] Heat at [80C] for 3 hours. Cool at room temperature and add 1 N aqueous hydrochloric acid (20 mL) and extract with ethyl acetate. Wash with saturated aqueous sodium bicarbonate and dry the remaining organic phase over sodium sulfate and concentrate under reduced pressure to provide (0.91 g, 83%) of an oil. Add (2-fluoro-4-nitro-phenyl) -methanol (0.91 g) to a mixture of dioxide manganese (1.1 g) in 20 ml of dichloromethane. Stir at room temperature overnight and filter over [CELITE@. ] Concentrate under reduced pressure to provide (0.27 g, 30%) of the title compound as an oil. |
With sulfur trioxide pyridine complex; triethylamine; In dimethyl sulfoxide; at 20℃; for 2h; | 43.3 g of 2-fluoro-4-nitrobenzoic acid was dissolved in 600 ml of dimethylformamide, and 1,1'-carbodiimide was added to it, and stirred at room temperature for 2 hours. 11.1 g of sodium borohydride was added thereto, and further stirred for 30 minutes. Aqueous saturated ammonium chloride solution was added to it, 800 ml of water was added thereto, extracted wit 1.2 liters of ethyl acetate, and the organic layer was washed with saturated saline water. The solvent was evaporated away under reduced pressure, the residue was again diluted with ethyl acetate, and the organic layer was washed with water and saturated saline water. This was dried with anhydrous sodium sulfate, and the solvent was evaporated away to obtain 32.7 g of a brown oil. The obtained oil was dissolved in 200 ml of dimethyl sulfoxide and 60 ml of triethylamine, and 88.7 g of sulfur trioxide/pyridine complex was gradually added to it, and stirred at room temperature for 2 hours. This was diluted with ethyl acetate, and the organic layer was washed with water, aqueous 0.1 N hydrochloric acid solution and saturated saline water. The solvent was evaporated away under reduced pressure, and the residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate) and through crystallization (methanol/diethyl ether) to obtain 14.0 g of the entitled compound as an orange solid. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
99% | With sodium tetrahydroborate; In methanol; at 20℃; for 0.25h; | To a solution of 2-fluoro-4-nitrobenzaldehyde (1.0 g, 5.92 mmol) in CH3OH (10 mL),NaBH4 (814 mg, 22 mmol) was added.After stirring at room temperature for 15 minutes, the mixture was concentrated.The residue was partitioned between EA (100 mL) and saturated brine (100 mL). The combined organic phases were washed with saturated brine (100 mL x 2) and dried over Na2SO4.Concentrate to give a red solid (2-fluoro-4-nitrophenyl)methanol (1.0 g, 99%). |
1 g | With sodium tetrahydroborate; In methanol; at 20℃; for 0.25h; | [0482] To a solution of 2-fluoro-4-nitrobenzaldehyde (1.0 g, 5.92 mmol) in CH30H (10 mL)was added NaBH4 (814 mg, 22 mmol). After stirring at RT for 15 min, the mixture wasconcentrated. The residue was partitioned between 100 mL of EA and 100 mL of brine. Thecombined organic layers were washed with brine (100 mL x 2), dried over Na2S04, andconcentrated to afford 1.0 g of (2-fluoro-4-nitrophenyl) methanol (99%) as a red solid. MS (ESI)m/e [M+It 172.0. |