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Preparation of lucigenine

   42.7 g of N-fenylanthranil acid is mixed with 100 ml of sulfuric acid of density 1.82 g cm -3 . Heat the mixture about 4 hours in a water bath (use chlorkalcine tube). Then gradually pour the mixture into the boiling water and the precipitate formed after five minutes, filter off. Remove traces of acid solution Na 2 CO 3 T.T acridone is 344-346 ° C, yield about 90%

   39 g acridine are dissolved in 200 ml flask, a small quantity of water with 8 g of NaOH and then added 0.2 mol of DMF (about 19 mL). After 2 hours of standing, the pH checked and if an alkaline reaction disappeared, the solution is boiled for about 1 hour under reflux with 20 ml of 20% KOH solution. After acidification with concentrated HCl is excreted N-methylakridon. N-methylakridon filter off and dry. 15 g of N-methylakridonu cook 30 minutes with 45 ml POCL 3 in an oil bath preheated to 120 ° C. Cooled mixture was stirred with ether and the separated 9-chloro-N-methylakridiniumdichloro-fosát is filtered and dried at room temperature. 7.5 g of Mg shavings are dissolved in 50 g bromobenzene and 200 ml of ether and all of 9-chloro-N-methylakridiniumdichloro-fosát gradually introduced into this solution. After the reaction is refluxed for 15 minutes. After pouring the mixture into 200 ml of 2M HCl under ice cooling, stirred for 15 minutes, then basified with aqueous NH 3 . Drops 12 g of N, N-dimethylakridinu. N, N-dimethylakridin filtered and simmer 3 hours with methanol and once from benzene. After filtration, the product is stirred with 450 ml of hot 1 M HNO 3 and filtered hot. After cooling to eliminate lucigenin nitrate as a yellow powder.
Yield: about 60%

Lucigenine - preparation

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