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CAS No. : | 619-66-9 | MDL No. : | MFCD00006951 |
Formula : | C8H6O3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | GOUHYARYYWKXHS-UHFFFAOYSA-N |
M.W : | 150.13 | Pubchem ID : | 12088 |
Synonyms : |
Tetraphthalaldehydic acid
|
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 1,1'-carbonyldiimidazole; In tetrahydrofuran; water; | EXAMPLE 6 p-Formyl-N,N-dimethylbenzamide benzylamidinohydrazone hydrochloride A mixture of 15.0 g. of 4-carboxybenzaldehyde, 17.0 g. of N,N'-carbonyldiimidazole and 150 ml. of tetrahydrofuran is allowed to stand at room temperature for one hour. Dimethylamine is passed thru the above solution for one hour and the reaction mixture is allowed to stand at room temperature for 18 hours, then is heated at reflux temperature for one hour. Water is added and the solvent is distilled off. The residue is extracted with methylenechloride. The organic layer is washed with dilute hydrochloric acid and water, dried over magnesium sulfate and concentrated to an oil. The oil is triturated with a little methylene chloride and the insoluble material is filtered off. The mother liquor is concentrated and 7.9 g. of p-formyl-N,N-dimethylbenzamide is obtained as an oil. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Example 278 4-[(2-Methoxy-5-phenylcarbamoyl-phenylamino)-methyl]-benzoic acid The title compound has been made using the procedure of Example 50, but using <strong>[120-35-4]3-amino-4-methoxy-benzanilide</strong> and 4carboxybenzaldehyde, which are available from Aldrich, as starting materials; mp >240 C. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
93.3% | With triethylamine; In ethanol; at 60℃; for 4h;Product distribution / selectivity; | To a solution of 4-formylbenzoic acid (250 mg, 1.67 mmol) in ethanol (5 mL) were added triethylamine (0.28 mL, 2.00 mmol) and <strong>[57497-39-9]N-tert-butylhydroxylamine hydrochloride</strong> (251 mg, 2.00 mmol). The mixture was then heated at 60° C. for 4 hours. The solvent was evaporated in vacuo and the residue purified by flash column chromatography on silica gel using 1percent acetic acid in ethyl acetate. The product was obtained as a white solid (320 mg, 1.56 mmol, 93.3percent). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
53% | To a suspension of 4-formylbenzoic acid (4.00 g, 26.7 mmol) in dry DCM (8 mL) were added thionyl chloride (2.92 g, 40.0 mmol) and DMF (0.6 mL) dropwise at ambient temperature under nitrogen. The reaction mixture was refluxed for 2 h. After cooling, this mixture was added to 33% dimethylamine in water (10.5 mL, 72 mmol) dropwise over 15 min in an ice-water bath, and the reaction mixture stirred for 1 h at the same temperature. The solvent was evaporated in vacuums. The residue was purified by chromatography on silica gel to give the title compound (2.5 g, yield 53%) as a yellow solid. 1H-NMR (400 MHz, DMSO-d6) delta (ppm): 2.86 (s, 3H), 3.30 (s, 3H), 7.60 (d, J=7.6 Hz, 2H), 7.95 (d, J=7.6 Hz, 2H), 10.04 (s, 1H); LC-MS (ESI) m/z: 178 (M+1)+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
53% | Example 101 A 4-Formyl-N,N-dimethylbenzamide[00685] To a suspension of 4-formylbenzoic acid (4.00 g, 26.7 mmol) in dry DCM (8 mL) were added thionyl chloride (2.92 g, 40.0 mmol) and DMF (0.6 mL) dropwise at ambient temperature under nitrogen. The reaction mixture was refluxed for 2 h. After cooling, this mixture was added to 33% dimethylamine in water (10.5 mL, 72 mmol) dropwise over 15 min in an ice-water bath, and the reaction mixture stirred for 1 h at the same temperature. The solvent was evaporated in vacuums. The residue was purified by chromatography on silica gel to give the title compound (2.5 g, yield 53%) as a yellow solid. ^-NMR (400 MHz, DMSO-i/6) 8(ppm): 2.86 (s, 3H), 3.30 (s, 3H), 7.60 (d, J= 7.6 Hz, 2H), 7.95 (d, J= 7.6 Hz, 2H), 10.04 (s, 1H); LC-MS (ESI) m/z: 178 (M+l)+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In ethanol; at 60℃; for 0.5h; | General procedure: A mixture of corresponding hydrazinylpyridazine 1 or 5 (1 mmol) and aldehyde 2 (1.1 mmol) in ethanol (5 mL) was heated at 60 oC for 0.5 h. The formation of hydrazone was checked by TLC and the reaction mixture was cooled to rt. Oxone (1.5 mmol) was added to the mixture at rt followed by tetramethyl ammonium bromide (0.2 mmol) and the resulting mixture was heated at 60 oC for another 5 h. The mixture was cooled to rt and extracted with dichloromethane (2 × 25 mL), dried over anhydrous sodium sulphate and concentrated to obtain a residue which was purified by column chromatography using hexane/ethyl acetate as eluent to furnish the desired triazolopyridazines 4 and 7. | |
In ethanol; at 60℃; for 0.5h; | General procedure: A mixture of corresponding hydrazinylpyridazine 1 or 5 (1 mmol) and aldehyde 2 (1.1 mmol) in ethanol (5 mL) was heated at 60 C for 0.5 h. The formation of hydrazone was checked by TLC and the reaction mixture was cooled to rt. Oxone (1.5 mmol) was added to the mixture at rt followed by tetramethyl ammonium bromide (0.2 mmol) and the resulting mixture was heated at 60 C for another 5 h. The mixture was cooled to rt and extracted with dichloromethane (2 × 25 mL), dried over anhydrous sodium sulfate and concentrated to obtain a residue which was purified by column chromatography using hexane/ethyl acetate as eluent to furnish the desired triazolopyridazines 4 and 7 (See reference no; 7 for supporting information). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With benzotriazol-1-ol; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; N-ethyl-N,N-diisopropylamine; In dichloromethane; at 0 - 20℃; for 12h; | [0909] To a solution of AB-2 (1 g, 6.66 mmol, 1 eq), EDCI (1.53 g, 7.99 mmol, 1.2 eq), HOBt (900.03 mg, 6.66 mmol, 1 eq) and DIEA (3.44 g, 26.64 mmol, 4.64 mL, 4 eq) in DCM (15 mL) was added N-methylmethanamine (814.73 mg, 9.99 mmol, 915.43 muL, 1.5 eq, HCl) at 0C. The mixture was stirred at 20C. for 12 h to give a red solution. The completion of reaction was detected by TLC and LCMS. The reaction solution was diluted with DCM (40 mL), then washed with sat. aqu. NaHCO3 (30 mL) and brine (30 mL). The organic layer was dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by column chromatography (SiO2, Petroleum ether/Ethyl acetate=10/1 to 1:1) to give AG-3 . |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With (benzotriazo-1-yloxy)tris(dimethylamino)phosphonium hexafluorophosphate; N-ethyl-N,N-diisopropylamine; In N,N-dimethyl-formamide; at 20℃; for 16.0h; | [0914] To a solution of AI-1 (500 mg, 3.33 mmol, 1 eq) in DMF (5 mL) were added AI-2 (546.01 mg, 3.26 mmol, 9.78e-1 eq, HCl), DIEA (1.29 g, 9.99 mmol, 1.74 mL, 3 eq) and BOP (1.77 g, 4.00 mmol, 1.2 eq). The mixture was stirred at 20C. for 16 h to give a yellow solution. LCMS and TLC (eluting with: PE/EtOAc=1/1) showed the reaction was completed. The reaction mixture was quenched with H2O (20 mL) and extracted with MTBE (30 mL3). The organic layers were dried over Na2SO4 and concentrated to give the crude product. The product was purified by a flash column (eluting with:PE/EtOAc=5% to 50%) to give AI-3 . |
[ 99-04-7 ]
3-Methylbenzoic acid(Flakes or Chunks or Granular)
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3-Methylbenzoic acid(Flakes or Chunks or Granular)
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