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CAS No. : | 397322-46-2 | MDL No. : | MFCD23701524 |
Formula : | C10H8BrN | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 222.08 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P280-P305+P351+P338-P310 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H332-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 |
---|---|---|
26% | With N-Bromosuccinimide; NaH In tetrahydrofuran; tetrachloromethane; water; toluene | (28-6) To a solution of the compound of Example 28-5 (194 mg) in carbon tetrachloride (5.0 mL) were added N-bromosuccinimide (156 mg) and 2,2'-azobis(isobutyronitrile) (16.3 mg) under nitrogen atmosphere, and the mixture was heated under reflux for 2 hours. The reaction solution was cooled to room temperature, and the insoluble materials were removed by filtration. The solvent was evaporated under reduced pressure to about 3 ml. Further, toluene was added thereto, and the mixture was evaporated under reduced pressure to about 3 mL. This procedure was repeated five times to give a solution of a crude bromo compound in toluene. Under nitrogen atmosphere, a solution of the compound of Reference Example 1 (158 mg) in THF (5.0 mL) was cooled to 0°C, and thereto was added 60 percent NaH (37.06 mg). Further, thereto was added the solution of the crude bromo compound in toluene, and the mixture was stirred at 50°C for 2 hours. The reaction solution was cooled to room temperature, and water was added to the mixture, and further extracted twice with ethyl acetate. The extract was washed with water and a saturated brine, dried over magnesium sulfate, filtered, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column (hexane / ethyl acetate =3/ 1 --> 1/1) to give the title compound (90.9 mg, 26 percent). 1H NMR (CDCl3, 400MHz) δ 8.79 (d, 1H, J=2.1Hz), 8.20 (d, 1H, J=2.1Hz), 8.04 (d, 1H, J=8.4Hz), 7.80 (d, 1H, J=7.5Hz), 7.70 (d, 2H, J=8.0Hz), 7.53 (dd, 1H, J=7.5, 8.4Hz), 7.23 (d, 2H, J=8.0Hz), 7.11 (dd, 1H, J=1.7, 2.5Hz), 6.86 (dd, 1H, J=1.7, 4.0Hz), 6.31 (dd, 1H, J=2.5, 4.0Hz), 5.91 (s, 2H), 2.41 (s, 3H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
26% | With N-Bromosuccinimide; NaH In tetrahydrofuran; tetrachloromethane; water; toluene | (28-6) To a solution of the compound of Example 28-5 (194 mg) in carbon tetrachloride (5.0 mL) were added N-bromosuccinimide (156 mg) and 2,2'-azobis(isobutyronitrile) (16.3 mg) under nitrogen atmosphere, and the mixture was heated under reflux for 2 hours. The reaction solution was cooled to room temperature, and the insoluble materials were removed by filtration. The solvent was evaporated under reduced pressure to about 3 ml. Further, toluene was added thereto, and the mixture was evaporated under reduced pressure to about 3 mL. This procedure was repeated five times to give a solution of a crude bromo compound in toluene. Under nitrogen atmosphere, a solution of the compound of Reference Example 1 (158 mg) in THF (5.0 mL) was cooled to 0° C., and thereto was added 60percent NaH (37.06 mg). Further, thereto was added the solution of the crude bromo compound in toluene, and the mixture was stirred at 50° C. for 2 hours. The reaction solution was cooled to room temperature, and water was added to the mixture, and further extracted twice with ethyl acetate. The extract was washed with water and a saturated brine, dried over magnesium sulfate, filtered, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column (hexane/ethyl acetate=3/1-->1/1) to give the title compound (90.9 mg, 26percent). 1H NMR (CDCl3, 400 MHz) δ 8.79 (d, 1H, J=2.1 Hz), 8.20 (d, 1H, J=2.1 Hz), 8.04 (d, 1H, J=8.4 Hz), 7.80 (d, 1H, J=7.5 Hz), 7.70 (d, 2H, J=8.0 Hz), 7.53 (dd, 1H, J=7.5, 8.4 Hz), 7.23 (d, 2H, J=8.0 Hz), 7.11 (dd, 1H, J=1.7, 2.5 Hz), 6.86 (dd, 1H, J=1.7, 4.0 Hz), 6.31 (dd, 1H, J=2.5, 4.0 Hz), 5.91 (s, 2H), 2.41 (s, 3H). |