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A suspension of 4-formylbenzenesulfonic acid sodium salt (1.0 g, 4.78 mM) in excess of thionylchloride (15 ml) was heated to reflux for 30 minutes. The mixture was then concentrated to dryness, dissolved in anhydrous THF (20 ml). The mixture was cooled (ice-bath) to which was added excess of ammonia (5 ml, 1.0M solution in THF) and the suspension was stirred for 3 hrs at ambient temperature. The reaction was quenched with ice-cold water where up on the amide precipitated out. It was filtered, washed with water and vacuum dried overnight. Efforts were not made to purify the amide and it was used as such in the subsequent reaction. The crude amide was dissolved in methanol (20 ml) and subjected to condensation with N-tert-butylhydroxylamine hydrochloride (0.72 g, 5.74 mM) at refluxing temperature for 6 hrs. Concentration of the mixture followed by silicagel column chromatography afforded the title compound as a white solid. MS: m/z 257 (MH+). 1H NMR delta 1.51(s, 9H); 7.39(brs, 2H); 7.83(d, J=8.8 Hz, 2H); 7.99(s, 1H); 8.49 (d, J=8.8 Hz, 2H).
General procedure: Porphyrins were prepared using the typical Adler reaction. Pyrrole (30 mmol) was slowly added to a mixture of substituted benzaldehyde (30 mmol) and propionic acid (105 mL) through a dropping funnel. The mixture was heated to 120-140 C for 1-3 h. After cooling, the reaction mixture was filtered, washed and dried under vacuum to obtain the crystal of porphyrins.
With sodium carbonate; In water; at 30℃; for 5.0h;
In a 250 ml three-necked flask equipped with a thermometer and a stirrer, 20 g of mequindoc, 21 g of sodium sulfonate benzaldehyde,Water 50ml, sodium carbonate 4.86g, 30 constant temperature stirring 5h, cooled to 0 , crystal Yang 1h, filtered, washed with acetone, dried to give waterSolvent Quinocetone 29.2g, yield 77.9%
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