Preparation method of indole-containing heterocycle pyridinedihydrofuranketone
A technology of indole heterocyclic pyridine and dihydrofuranone, which is applied in the field of preparation of pyridodihydrofuranone compounds, can solve the problems of low yield, slow solidification speed of crude products, consumption of lye, etc., and achieve high yield, The effect of less solvent amount and easy post-treatment
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Embodiment 1
[0016] Add 60 grams of quinolinic anhydride, 120 grams of 2-methyl-1-n-octylindole and 120 mL of toluene into a 500 mL three-necked flask, stir and heat up to 50 ° C, react at this temperature for 5 hours, cool to room temperature, and add 120 mL Anhydrous ethanol, stir evenly, refrigerate at 0-5°C for 5 hours, filter, rinse the filtrate with a small amount of absolute ethanol, rinse with petroleum ether (I) until the filtrate is light in color, and dry at room temperature to obtain 108 g Light yellow solid, melting point: 121°C (decomposition), yield: 68%.
[0017] Add 39.2 g of the obtained intermediate and 23.8 g of 3-N, N-dipropylaminoacetanilide into a 500 mL three-necked flask, add 80 mL of acetic anhydride, react at 40 ° C for 5 hours, cool slightly, and add 160 mL of anhydrous Ethanol, refrigerated overnight at 0-5°C, filtered the next day, rinsed the filter cake with cold ethanol, drained, and recrystallized the crude product with absolute ethanol to obtain 40.2 g of ...
Embodiment 2
[0022] Add 60 grams of quinolinic anhydride, 120 grams of 2-methyl-1-n-octylindole and 120 mL of benzene into a 500 mL three-necked flask, stir and heat up to 70 ° C, react at this temperature for 4 hours, cool to room temperature, and add 150 mL Methanol, stirred evenly, refrigerated at 0-5°C for 5 hours, filtered, and the filtrate was rinsed with a small amount of methanol, and then rinsed with petroleum ether (I) until the filtrate was light in color, and dried at room temperature to obtain 99 grams of a light yellow solid. Melting point: 121°C (decomposition), yield: 63%.
[0023] Add 39.2 g of the obtained intermediate and 23.8 g of 3-N,N-dipropylaminoacetanilide into a 500 mL three-necked flask, add 100 mL of acetic anhydride, react at 50°C for 4 hours, cool slightly, and add 160 mL of isopropanol while stirring , refrigerated overnight at 0-5°C, filtered the next day, rinsed the filter cake with cold isopropanol, drained, and recrystallized the crude product with absolu...
Embodiment 3
[0028] Add 60 grams of quinolinic anhydride, 120 grams of 2-methyl-1-n-octylindole and 120 mL of chlorobenzene into a 500 mL three-necked flask, stir and heat up to 90 ° C, react at this temperature for 3 hours, cool to room temperature, add 120mL isopropanol, stir well, refrigerate at 0-5°C for 5 hours, filter, rinse the filtrate with a small amount of isopropanol, rinse with petroleum ether (I) until the color of the filtrate is light, and dry at room temperature to obtain 93 g light yellow solid, melting point: 121°C (decomposition), yield: 58%.
[0029] Add 39.2 grams of the obtained intermediate and 23.8 grams of 3-N,N-dipropylaminoacetanilide into a 500 mL three-necked flask, add 80 mL of acetic anhydride, react at 60 ° C for 3 hours, cool slightly, and add 160 mL of absolute ethanol while stirring , refrigerated overnight at 0-5°C, filtered the next day, rinsed the filter cake with cold ethanol, and drained, and recrystallized the crude product with absolute ethanol to ...
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