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CAS No. : | 400-74-8 | MDL No. : | MFCD00024576 |
Formula : | C7H3F4NO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | DNTHMWUMRGOJRY-UHFFFAOYSA-N |
M.W : | 209.10 | Pubchem ID : | 94954 |
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: |
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* 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 |
---|---|---|
With potassium carbonate; In acetonitrile; at 80.0℃; | 1-Fluoro-4-nitro-2- (trifluoromethyl) benzene(300 mg, 1.4 mmol), (R) - (+) - 3-dimethylaminopyrrolidine dihydrochloride(261 mg, 1.4 mmol) was dissolved in acetonitrile (20 mL) and potassium carbonate (387 mg, 2.8 mmol) was added. The reaction system at 80 C overnight, then allowed to cool. The reaction mixture was poured into water (10 mL) and extracted with ethyl acetate (3 x 20 mL). The organic phase is collected, dried over Na2SO4, filtered and concentrated to dryness. The crude title compound (320 mg) was used as a yellow solid for the next reaction. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
39% | With potassium carbonate; In dimethyl sulfoxide; at 20℃; for 1.0h; | A solution of 1-fluoro-4-nitro-2-(trifluoromethyl)benzene (5.3 mL, 38 mmol) and <strong>[74420-02-3]1H-pyrrolo[2,3-b]pyridin-4-ol</strong> (CAS No. [74420-02-3]; 4.67 g, 34.8 mmol) in DMSO (110 mL) was treated withpotassium carbonate (19.2 g, 139 mmol) and stirred at room temperature for 1 hour. The reaction mixture was diluted with ethyl acetate (200 mL) and washed with two times with 20 mL water and brine (20 mL), dried with sodium sulfate and concentrated in vacuo. The resulting residue was purified via a Biotage chromatography system (bOg snap KP-Silcolumn, hexane I 20 ? 100percent ethyl acetate) to obtain 4.62 g (96 percent purity, 39 percent yield) of thedesired title compound.1HNMR (400 MHz, DMSO-d6) delta [ppm]: 6.11 (d, 1H), 6.92 (d, 1H), 7.25 (d, 1H), 7.48 (d, 1H),8.28 (d, 1 H), 8.46 (dd, 1 H), 8.58 (d, 1 H), 12.05 (br s, 1 H). |
39% | With potassium carbonate; In dimethyl sulfoxide; at 20℃; for 1.0h; | A solution of 1 -fluoro-4-nitro-2-(trifluoromethyl)benzene (5.3 mL, 38 mmol) and 1 /-/-pyrrolo[2,3- b]pyridin-4-ol (CAS No. [74420-02-3]; 4.67 g, 34.8 mmol) in DMSO (1 10 mL) was treated with potassium carbonate (19.2 g, 139 mmol) and stirred at room temperature for 1 hour. The reaction mixture was diluted with ethyl acetate (200 mL) and washed with two times with 20 mL water and brine (20 mL), dried with sodium sulfate and concentrated in vacuo. The resulting residue was purified via a Biotage chromatography system (100g snap KP-Sil column, hexane / 20 - 100percent ethyl acetate) to obtain 4.62 g (96 percent purity, 39 percent yield) of the desired title compound. 1H-NMR (400 MHz, DMSO-d6) delta [ppm]: 6.1 1 (d, 1 H), 6.92 (d, 1 H), 7.25 (d, 1 H), 7.48 (d, 1 H), 8.28 (d, 1 H), 8.46 (dd, 1 H), 8.58 (d, 1 H), 12.05 (br s, 1 H). |
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