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CAS No. : | 17100-63-9 | MDL No. : | MFCD08436018 |
Formula : | C9H9BrO3 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | XLKDKHRGIJWOSN-UHFFFAOYSA-N |
M.W : | 245.07 | Pubchem ID : | 14570117 |
Synonyms : |
|
Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H315-H319-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 |
---|---|---|
65.38% | To the solution of <strong>[42182-27-4]2-aminoisonicotinonitrile</strong> (1.4g, 11.75mmol) in toluene (60mL) was added Al(Me)3 (5.87ml, 11.75mmol) at room tempereture. After stiring for 30min, methyl 4-bromo-3-methoxybenzoate (2.88g, 11.75mmol) was added. The reaction was refluxed for 3h. The mixture was quenched with IN HC1 and partitioned with H20 (45 mL) and EA (10 mL*3). The EA layer was dried, filtered, concentrated, and purified by column chromatography on silica gel (PE: EA = 0-60percent) to give 4-bromo-N-(4- cyanopyridin-2-yl)-3-methoxybenzamide (2.55g, 65.38percent>) as a white solid. 1H NMR (400MHz, CDCls) delta= 8.69 (s, 1H), 8.65 (br. s., 1H), 8.49 (dd, J=0.8, 5.0 Hz, 1H), 7.69 (d, J=8.0 Hz, 1H), 7.51 (d, J=2.0 Hz, 1H), 7.33 - 7.29 (m, 2H), 4.01 (s, 3H). | |
65.38% | (a) 4-bromo-N-(4-cyanopyridin-2-yl)-3-methoxybenzamide To the solution of <strong>[42182-27-4]2-aminoisonicotinonitrile</strong> (1.4 g, 11.75 mmol) in toluene (60 mL) was added Al(Me)3 (5.87 ml, 11.75 mmol) at room temperature. After stirring for 30 min, methyl 4-bromo-3-methoxybenzoate (2.88 g, 11.75 mmol) was added. The reaction was refluxed for 3 h. The mixture was quenched with 1N HCl and partitioned with H2O (45 mL) and EA (10 mL*3). The EA layer was dried, filtered, concentrated, and purified by column chromatography on silica gel (PE: EA=0-60percent) to give 4-bromo-N-(4-cyanopyridin-2-yl)-3-methoxybenzamide (2.55 g, 65.38percent) as a white solid. 1H NMR (400 MHz, CDCl3) delta=8.69 (s, 1H), 8.65 (br. s., 1H), 8.49 (dd, J=0.8, 5.0 Hz, 1H), 7.69 (d, J=8.0 Hz, 1H), 7.51 (d, J=2.0 Hz, 1H), 7.33-7.29 (m, 2H), 4.01 (s, 3H). | |
65.38% | To the solution of <strong>[42182-27-4]2-aminoisonicotinonitrile</strong> (1.4g, 11.75mmol) in toluene (60mL) was added Al(Me)3 (5.87ml, 11.75mmol) at room tempereture. After stiring for 30min, methyl 4-bromo-3-methoxybenzoate (2.88g, 11.75mmol) was added. The reaction was refluxed for 3h. The mixture was quenched with IN HCl and partitioned with H20 (45 mL) and EA (10 mL*3). The EA layer was dried, filterted, concentrated, and purified by column chromatography on silica gel (PE: EA = 0-60percent) to give 4-bromo-N-(4- cyanopyridin-2-yl)-3-methoxybenzamide (2.55g, 65.38percent) as a white solid. 1H NMR (400MHz, CDC13 ) delta = 8.69 (s, 1H), 8.65 (br. s., 1H), 8.49 (dd, J=0.8, 5.0 Hz, 1H), 7.69 (d, J=8.0 Hz, 1H), 7.51 (d, J=2.0 Hz, 1H), 7.33 - 7.29 (m, 2H), 4.01 (s, 3H). |
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