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CAS No. : | 194853-86-6 | MDL No. : | MFCD00061283 |
Formula : | C8H3F4N | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | LCCPQUYXMFXCAC-UHFFFAOYSA-N |
M.W : | 189.11 | Pubchem ID : | 605085 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P301+P312+P330 | UN#: | |
Hazard Statements: | H302 | 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 |
---|---|---|
41.27% | With sodium hydride; In N,N-dimethyl-formamide; at 0 - 20℃; for 16h; | Example 29 (+-)-4-[1-(4-Cyano-3-trifluoromethyl-phenoxy)-ethyl]-benzoic Acid Methyl Ester (+-)-4-[1-(4-cyano-3-trifluoromethyl-phenoxy)-ethyl]-benzoic acid methyl ester was prepared as follows: To a cooled solution (0 C.) of methyl-4-(1-hydroxyethyl)benzoate (1.00 g, 5.549 mmol) and 4-fluoro-2-(trifluoromethyl)benzonitrile (1.049 g, 5.549 mmol) in anhydrous dimethylformamide (8 mL) was added NaH (0.222 g as a 60% dispersion in mineral oil). The reaction mixture was allowed to warm to room temperature and was then stirred under nitrogen for 16 hr. The crude reaction mixture was added to ethyl acetate (150 ml) and was washed with saturated aqueous ammonium chloride (2*150 mL), water (1*150 mL), and saturated aqueous sodium chloride (1*150 mL). The organic layer was dried over anhydrous magnesium sulfate, filtered and concentrated. The crude material was chromatographed using hexanes and ethyl acetate (4:1) to afford 0.800 g (41.27% yield) of a viscous colorless oil; 1H NMR (400 MHz; CDCl3) delta 8.03 (d, 2H, J=8.3 Hz), 7.63 (d, 1H, J=8.3 Hz), 7.40 (d, 2H, J=8.3 Hz), 7.26 (apparent s occluded by solvent, 1H), 6.97 (dd, 1H, J=8.54, 2.44 Hz), 5.43 (q, 1H, J=6.34 Hz), 3.90 (s, 3H), 1.69 (d, 3H, 6.34 Hz); MS (APCI+) 373.1 ([M+1]+Na); CHN theoretical/actual: C, 61.89/61.90, H, 4.04/4.02, N, 4.01/3.94, F 16.32/16.20. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
60% | With sodium hydride; In dimethyl sulfoxide; mineral oil; at 20℃; for 1h; | Trans-cyclohexane-l,4-diol (4.30 mmol) and sodium hydride (60percent suspension in oil, 2.15 mmol) are suspended in dry dimethylsulfoxide (4 mL) and a solution of 4-fluoro-2-trifluoromethyl-benzonitrile (2.15 mmol) in dry dimethylsulfoxide (4 mL) is added dropwise. The resulting mixture is stirred at room temperature. After 1 hour reaction time, the reaction is treated with water (10 mL), the precipitate formed is separated by filtration and the filtrate is extracted with dichloromethane (25 mL). The organic phase is washed with aqueous saturated ammonium chloride (5 mL), dried over magnesium sulfate, filtered and the filtrate is concentrated under reduced pressure. The precipitate is triturated with diethylether (15 mL), filtered and the filtrate concentrated under reduced pressure. Both fractions of crude product are combined, dissolved in dichloromethane and purified by chromatography through a short pad of silica gel (dichloromethane and then diethylether as eluents) to afford the desired product (60percent yield). |
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