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CAS No. : | 4467-07-6 | MDL No. : | MFCD05864807 |
Formula : | C12H9NO2 | Boiling Point : | No data available |
Linear Structure Formula : | HOOCC6H4C5H4N | InChI Key : | IRXFQXMHMRTLIR-UHFFFAOYSA-N |
M.W : | 199.21 | Pubchem ID : | 5152592 |
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 |
---|---|---|
85% | With potassium carbonate;bis-triphenylphosphine-palladium(II) chloride; In water; acetonitrile; at 100℃; for 24.0h;Inert atmosphere; | Example 161 A3-(pyridin-2-yl)benzoic acid; To a solution of 3-boronobenzoic acid (1.66 g, 10 mmol) and 2-bromopyridine (1.72 g, 11 mmol) in acetonitrile (40 mL) and water (40 mL), potassium carbonate (5.5 g, 40 mmol), Bis(triphenylphosphine)palladium(II)chloride (400 mg, 0.37 mmol) was added. The mixture was degassed and purged withed nitrogen. The mixture was stirred at 100 C. for 24 h. Then the hot suspension was filtered and concentrated to half of the original volume and washed with dichloromethane. The aquatic phase was adjusted to pH=3 with hydrochloric acid (1 M) and filtrated, washed with water. The residue was dried in vacuum to obtain 1.69 g of white solid of 3-(pyridin-2-yl)benzoic acid. Yield: 85%. LC-MS (ESI) m/z: 200 (M+1)+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With thionyl chloride;Reflux; | Example 161 Bmethyl 2-hydroxy-3-(3-(pyridin-2-yl)benzamido)benzoate; Thionyl chloride (10 mL) was added to <strong>[4467-07-6]3-(pyridin-2-yl)benzoic acid</strong> (1.69 g, 8.5 mmol) and the mixture was stirred under reflux overnight. The solvent was evaporated under reduced pressure and the residue was dried in vacuum to give 3-(pyridin-2-yl)benzoyl chloride. 1.66 g of crude product was obtained. To a solution of methyl 3-amino-2-hydroxybenzoate (0.84 g, 5 mmol) and pyridine (790 mg, 10 mmol) in toluene (50 mL) were added crude 3-(pyridin-2-yl)benzoyl chloride (1.6 g, 7.37 mmol) portion-wise at 0 C. and then stirred at 70 C. for 4 h. The resulting mixture was extracted with ethyl acetate (100 mL×4), the organic phase was washed with water and saturated sodium bicarbonate, dried with anhydrous sodium sulfate and evaporated under reduced pressure to obtain yellow solid of methyl 2-hydroxy-3-(3-(pyridin-2-yl)benzamido)benzoate (1.48 g, yield 85%). LC-MS (ESI) m/z: 349 (M+1)+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
19% | To a flask containing 95 mg (0.48 mmol) of <strong>[4467-07-6]3-(pyridin-2-yl)benzoic acid</strong> and 20 mg (0.50 mmol) of NaOH was added 30 mL of degassed aqueous methanol solution (Fi20:MeOH 1 :5 v/v). The reagents were stirred until all components were dissolved and then transferred to a flask containing 188 mg (0.362 mmol) of Ru(bpy)2Cl2 and 180 mg (0.93 mmol) AgBF4. The reaction mixture was heated at reflux for 18 hrs, cooled, and then filtered through celite to afford a dark red/purple filtrate. The solvent was removed in vacuo and then passed through a silica column (MeCN:KN03(aq) 7: 1 v/v), followed by anion exchange with a saturated aqueous NH4PF methanolic solution to produce 52 mg of a red precipitate (yield = 19%). NMR (CD3CN): 6.61 (d, 1H, J = 8 Hz), 6.98 (dt, 1H, J = 7 Hz, 6 Hz, l = 1 Hz), 7.17-7.25 (m, 3H), 7.39, (dd, 1H, J = 8 Hz, l = 2 Hz), 7.42 (dt, 1H, J = 8 Hz, l = 1 Hz), 7.60 (d, 1H, J = 5 Hz), 7.69-7.75 (m, 3H), 7.78-7.87 (m, 4H), 7.95 (d, 1H, 3 J = 6 Hz), 7.99 (dt, 1H, J = 8 Hz, J = 2 Hz), 8.14 (d, 1H, J = 8 Hz), 8.31 (d, 1H, J = 7 Hz), 8.33 (d, 1H, J = 7 Hz), 8.38 (d, 1H, J = 8 Hz), 8.41 (d, 1H, l = 2 Hz), 8.46 (d, 1H, J = 8 Hz), 9.08 (vbr, 1H). ESI-MS: m/z, 612.1 (calcd for {M+} 612.1) Anal. Calcd. for C32H24F6N5O2PRU + 0.5 H20: C, 50.20; H, 3.29; N, 9.15. Found: C, 50.29; H, 3.49; N, 9.07. |