New derivatives of benzo[a]pyrano[3,2-h]acridin-7-one, a process for their preparation and pharmaceutical compounds containing them
A technology of compounds and medicinal acids, applied in the field of novel benzo[a]pyrano[3, which can solve the problems of low potency, limited bioavailability, low solubility, etc.
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Embodiment 1
[0356] Example 1: 6-Hydroxy-3,3-dimethyl-3,14-dihydro-7H-benzo[a]pyrano[3,2-h]acridin-7-one
[0357] 732 mg of the compound of Preparation 2 was dissolved in 20 ml of anhydrous dimethylformamide, and then 732 mg of anhydrous potassium carbonate was added. The mixture thus obtained was stirred under argon at 65° C. for 15 minutes, then 876.5 mg of anhydrous potassium iodide and 2.47 g of 3-chloro-3-methyl-1-butyne were added. At the end of 5 hours, the reaction mixture was heated at 130° C. for 2 hours to rearrange the propargyl ether. Then, the reaction mixture was diluted with 50ml of water and extracted with dichloromethane (3 x 40ml). The combined organic phases were washed with water and then with 1M potassium hydroxide solution, dried over anhydrous sodium sulfate, filtered and evaporated to dryness under reduced pressure. By silica gel chromatography (cyclohexane followed by a gradient of 1-5% acetone / cyclohexane), 326 mg of the desired product could be isolated.
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Embodiment 2
[0359] Example 2: 6-Hydroxy-3,3,14-trimethyl-3,14-dihydro-7H-benzo[a]pyrano[3,2-h]acridin-7-one
[0360] 1.324 g of sodium carbonate were added to 411.6 mg of the compound of Example 1 dissolved in 50 ml of dry acetone. The mixture was kept under argon atmosphere at 0° C. for 15 minutes with stirring, then after the addition of 852 mg of methyl iodide, the reaction mixture was heated to reflux for 2 hours. After cooling, excess methyl iodide was destroyed by adding 40 ml methanol and 50 ml water. Methanol was distilled off and the aqueous phase was extracted with dichloromethane (3 x 30ml). The combined organic phases were washed with 10% aqueous NaOH, then water, dried over anhydrous sodium sulfate, then filtered and evaporated to dryness under reduced pressure. By chromatography on silica gel (cyclohexane followed by a gradient of 0.5-5% acetone / cyclohexane), 374.2 mg of the desired product were isolated.
[0361] Mass spectrometry (DIC / NH 3 ): m / z=358(M+H) +
Embodiment 3
[0362] Example 3: 6-methoxy-3,3,14-trimethyl-3,14-dihydro-7H-benzo[a]pyrano[3,2-h]acridin-7-one
[0363] A solution of 604.3 mg of the compound of Example 2 in 40 ml of anhydrous acetone was gradually added to a suspension of 61 mg of sodium hydride in 10 ml of acetone maintained at 0°C under an argon atmosphere. The mixture thus obtained was kept at 0° C. for 30 minutes, and then 1.2 g of methyl iodide were added. The reaction mixture was heated to reflux for 6 hours. After cooling, excess methyl iodide was destroyed by adding 40 ml methanol and 50 ml water. Methanol was distilled off and the aqueous phase was extracted with dichloromethane (3 x 30ml). The combined organic phases were washed with 10% aqueous NaOH, then water, dried over anhydrous sodium sulfate, then filtered and evaporated to dryness under reduced pressure. Chromatography on silica gel (cyclohexane followed by a gradient of 1-10% acetone / cyclohexane) yielded 469.5 mg of the desired product.
[0364] Mass...
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