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Step 3: 2-Amino-3-nitro-benzoic acid; To a ice cold solution of 7-nitro-1 H-indole-2,3-dione (9 g, 47 mmol) in 2 M aqueous sodium hydroxide (50 ml_), 30% hydrogen peroxide (9 ml.) was added drop wise. The mixture was warmed to room temperature and stirred overnight. The mixture was carefully acidified by addition of a saturated citric acid solution. The solid precipitate was collected by filtration, washed with water and dried in a vacuum oven to get 6 g of the required product as a yellow coloured solid (70%).1H NMR (300 MHz, DMSOd6): delta (ppm) = 8.9(br.s, 1 H), 8.19(m, 2H), 6.63(m, 1 H). HPLC purity: 98 %. LCMC(-ive mode): 93% and m/z:181.9
With magnesium(II) perchlorate; In ethanol; water; at 50℃; for 0.5h;
General procedure: Mg(ClO4)2 (10 mol %) was added to a mixture of isatin (2 mmol), malononitrile or ethyl cyanoacetate (2mmol), and dimedone (2 mmol) in aqueous ethanol solution(50%, v/v, 5 mL), and the resulting mixture was stirred at 50C for 30-60 min. Upon completion of the reaction (TLC),the mixture was allowed to cool to room temperature. The resulting solid was filtered and washed successively with water (2 × 30 mL) and cold aqueous ethanol (2 × 1 mL) to afford pure product 4.
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