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CAS No. : | 579-75-9 | MDL No. : | MFCD00002431 |
Formula : | C8H8O3 | Boiling Point : | - |
Linear Structure Formula : | (CH3O)C6H4COOH | InChI Key : | ILUJQPXNXACGAN-UHFFFAOYSA-N |
M.W : | 152.15 | Pubchem ID : | 11370 |
Synonyms : |
NSC 3778;O-Methylsalicylic acid;Salicylic acid methyl ether
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338 | 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 |
---|---|---|
With potassium hydroxide; In ethylene glycol; at 170℃; for 7h; | General procedure: 2-Ethylbenzonitrile (7.6mmol) and KOH (24.8mmol) were suspended in ethane-1,2-diol (10mL) and stirred at 170C for 7h. Then, the reaction mixture was cooled down to rt, H2O (50mL) was added and the resulting mixture was extracted three times with ether (30mL). pH of the aqueous layer was adjusted to 1 by diluted HCl and the aqueous phase was extracted three times with ether (40mL). Organic phases were collected, extracted three times with H2O (40mL) and dried over Na2SO4. The solvent was removed and obtained compound was directly used in the next step. Yield: 89.0%, white solid; mp: 64-65C; IR: 3400-2300 (b, OH), 2977 (as CH3), 2955 (as CH2), 2869 (s CH3), 1681 ( CO), 1601, 1575, 1488, 1447 ( CC aromatic) cm-1; 1H NMR (DMSO-d6, 300MHz): δ 12.79 (1H, br s, COOH), 7.76 (1H, d, J=7.0Hz), 7.43 (1H, t, J=7.5Hz), 7.33-7.21 (2H, m), 2.90 (2H, q, J=7.4Hz, CH2), 1.14 (3H, t, J=7.4Hz, CH3); 13C NMR (DMSO-d6, 75MHz): δ 169.14, 145.12, 131.96, 130.54, 130.35, 130.34, 126.04, 27.03, 16.32. | |
With water; at 100℃; | After adding 16.2 g of 30% sodium methoxide and 0.1 mol of o-chlorobenzonitrile to a 100 ml autoclave, the air was replaced with nitrogen three times.Seal the reaction kettle, heat up to 100 120 , the reaction pressure is about 0.3Mpa 0.5Mpa, and keep it for 2 hours to 4 hours.HPLC analysis of o-chlorobenzonitrile 14.7 g of 30% liquid alkali was added dropwise, and the methanol was recovered by heating and distillation. When the internal temperature reached 100 C, it was converted to reflux.The reaction was maintained at reflux for 2 hours to 8 hours. When the <strong>[6609-56-9]o-methoxybenzonitrile</strong> was less than 0.5% as the end point, the reaction solution was cooled, and the pH was adjusted to 4 with hydrochloric acid.A large amount of white solid was precipitated, filtered, washed with water, and dried to obtain o-methoxybenzoic acid. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
100% | With N-ethyl-N,N-diisopropylamine; HATU; In N,N-dimethyl-formamide; at 20℃; for 24h; | (3) Synthesis of tert-Butyl 3-[(2-methoxy benzoyl)amino]methyl}piperidine-1-carboxylate HATU (293 mg, 0.77 mmol) was added to a DMF (3 mL) solution of the compound (150 mg, 0.7 mmol) synthesised in (2), 2-methoxybenzoic acid (117 mg, 0.77 mmol), and diisopropylethylamine (0.27 mL,1.54 mmol), and the mixture was stirred at room temperature for 24 hours. After adding ethyl acetate, the reaction mixture was washed twice with distilled water, and once with saturated brine. The organic layer was dried over magnesium sulfate, and concentrated under reduced pressure. The resulting residue was then purified using silica gel column chromatography to obtain the target (244 mg, 100percent). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
General procedure: To a solution of 3a (1 g) in ethanol was added Pd/C (5%, 0.1 g) and the mixture was stirred for 24 hrs at room temperature in a hydrogen atmosphere under atmospheric pressure. Insoluble matters were removed using Celite, and the filtrate was concentrated in vacuo to give the desired product 4a (0.76 g) as a yellow solid. To a solution of carboxylic acid (1 equiv) in CH2Cl2 (15 mL) at 0 C was added DMAP (1 equiv) and EDCI (1 equiv). The reaction mixture was stirred at 0 C for 45 minutes. At this time 4a (1 equiv) was added and the mixture was warmed to room temperature and stirred overnight. The resulting mixture was concentrated in vacuo, partitioned between 1.0 M HCl (20 ml) and ethyl acetate (3×20 mL). The combined organic layers were washed with brine (2 × 15 ml), dried over Na2SO4, filtered and concentrated in vacuo. The crude residue was purified by silica gel chromatograph using a mixture of petroleum ether/ethyl acetate (20 : 5, v/v) as eluent to afford the product as a white solid. To a solution of the obtained solid (1 equiv) in 2:3:1 THF/MeOH/H2O (18 ml) was added LiOH·H2O (1.5 equiv). After stirring at room temperature for 4 h, the volatiles were removed under reduced pressure. The residue was acidified with 1N hydrochloric acid solution, and then filtered and the filter cake was washed with 5 mL of water, dried in vacuum to afford a white powder. Recrystallization from 75% EtOH gave the desired compounds 2-17 as white solid. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
3.51 mmol | With 2,4,6-tripropyl-1,3,5,2,4,6-trioxatriphosphinane-2,4,6-trioxide; N-ethyl-N,N-diisopropylamine; In tetrahydrofuran; ethyl acetate; at 80℃; for 18h;Inert atmosphere; | A solution of <strong>[112734-22-2](4-bromo-2-fluoro-phenyl)methanamine</strong> (5.00mmol) in THF (4 mL), a propylphosphonic anhydride solution(50 wtpercent in EtOAc, 7.50 mmol) in THF (6 mL), 2-methoxy-5-methylbenzoic acid (6.04 mmol), and N,Ndiisopropylethylamine (8.88 mmol) was stirred at 80 °C for 18 h. The reaction was cooled to RT and partitioned between EtOAc and a saturated aqueous solution of NH4CI. The organic layer was washed with brine, dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified to give the titled compound (3.51 mmol). UPLC-MS (ES, Short acidic): 2.05 mi m/z 353.9 [M+2] |
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