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CAS No. : | 2144-08-3 | MDL No. : | MFCD00003325 |
Formula : | C7H6O4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | CRPNQSVBEWWHIJ-UHFFFAOYSA-N |
M.W : | 154.12 | Pubchem ID : | 75064 |
Synonyms : |
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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: |
* 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 |
---|---|---|
91.6% | With sulfuric acid; acetic acid; | 7,8-Dihydroxy-2-(4-dimethylaminostyryl)-1-benzopyrylium hydrogen sulfate was prepared from condensation of 2,3,4-trihydroxybenzaldehyde (3 mmol, 0.46 g) with <strong>[5432-53-1]p-dimethylaminostyryl methyl ketone</strong> [9] (3 mmol, 0.57 g). The reagents were dissolved in 8 ml of acetic acid and 2 ml of H2SO4. The reaction mixture was stirred overnight. By the following day ethyl acetate was added and a dark solid precipitated, was filtered off and carefully washed with ethyl acetate and dried yielding 1.12 g of 7,8-dihydroxy-2-(4-dimethylaminostyryl)-1-benzopyrylium hydrogen sulfate (2.75 mmol, 91.6%). 1H NMR (DCl/CD3OD, pD ? 1.0, 400.13 MHz) delta (ppm): 8.84 (1H, d, H4, 3JH4-H3 = 8.6 Hz); 8.55 (1H, d, Hbeta, 3JHbeta-Halpha = 15.6 Hz); 7.99 (2H, d, H2', H6', 3JH2',H6'-H3',H5' = 8.9 Hz); 7.79 (1H, d, H3, 3JH3-H4 = 8.6 Hz); 7.63 (1H, d, H5, 3JH5-H6 = 8.8 Hz); 7.52 (1H, d, Halpha, 3JHalpha-Hbeta = 15.6 Hz); 7.48 (2H, d, H3', H5', 3JH3',H5'-H2',H6' = 8.9 Hz); 7.38 (1H, d, H6, 3JH6-H5 = 8.8 Hz); 3.29 (6H, s, N(CH3)2. 13C NMR (DCl/CD3OD, pD ? 1.0) delta (ppm): 171.89; 157.75; 153.16 (C4); 151.07; 150.66; 149.71 (Cbeta); 147.48; 134.41; 134.02 (C2', C6'); 124.02 (C5); 120.86; 120.60 (C6); 119.5 (C3', C5'); 116.86 (C3); 44.53 . MS-MALDI/TOF+: calcd for C16H13O2+: 308.13 (100%); found: 308.07 [M]+ (100%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
83% | With potassium acetate; for 16h;Reflux; Inert atmosphere; | General procedure: Compounds were synthesized under anhydrous conditions, using a material previously dried at 60 C for at least 12 h and at 300 C for a few minutes immediately before use. A solution containing anhydrous CH3CO2K (2.94 mmol), the corresponding thiophenylacetic acid (1.67 mmol) and the corresponding hydroxysalicylaldehyde (1.67 mmol), in Ac2O (1.2 mL), was refluxed for 16 h. The reaction mixture was cooled, neutralized with 10% aqueous NaHCO3, and extracted with EtOAc (3 × 30 mL). The organic layers were combined, washed with water, dried over anhydrous Na2SO4 and the solvent was evaporated under reduced pressure. The product was purified by recrystallization in EtOH and dried in vacuum to afford the desired compound [26,27]. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With sodium metabisulfite; In ethanol; water; for 24h;Reflux; | General procedure: To a solution of the appropriate 3,4-diaminobenzene derivative (1ad)(2 mmol) in ethanol (15 mL) 2.85 N aqueous solution of sodium metabisulphite (1.6 mL) and the appropriate substituted arylaldehyde(2 mmol) were added. The reaction mixture was heated at reflux for 24 h. The solvent was then evaporated under reduced pressure. The residue was added with HCl 1 N (10 mL), the formed precipitate was filtered off, washed with water (3×10 mL) and purified by crystallization from the adequate solvent to give the title compounds.Following the general procedure benzimidazoles 3 [19], 4 [20], 5 [21],7 [24], 6, 32 and 33 [15] were prepared and their analytical and spectral data are in agreement with those reported in literature. |
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