Process for preparing alfuzosin hydrochloride
A technology for alfuzosin hydrochloride and an organic base, which is applied in the field of preparation of alfuzosin hydrochloride, can solve problems such as difficulty in realizing large-scale industrial production of alfuzosin hydrochloride, and achieves easy realization of reaction conditions, simplified operation, and reduced The effect of three waste pollution
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Embodiment 1
[0016] Embodiment 1: the preparation of alfuzosin hydrochloride
[0017] In a 3000 ml three-neck flask with mechanical stirring, add 1800 ml of chloroform and 82 ml of triethylamine, stir, cool down to 0°C in an ice-water bath, add 88 g of N-methylpropylenediamine and 134.5 g of 2-tetrahydrofuran Formyl chloride was reacted at room temperature for 18 hours, then 245.5 g of 2-chloro-4-amino-6,7-dimethoxyquinazoline was added, the temperature was controlled at 35-40°C, and the reaction was continued for 12 hours. After the reaction, wash with 1000 ml × 2 water, 800 ml 5% NaHCO 3 Washing with aqueous solution, washing with 800 ml saturated brine, anhydrous Na 2 SO 4 dry. After the solvent was evaporated under reduced pressure, it was dissolved in 1500 ml of absolute ethanol, and 380 ml of absolute ethanol-hydrogen chloride solution was added, stirred evenly, and placed for crystallization. Suction filtration and drying to obtain a white crystalline solid, which was recrystall...
Embodiment 2
[0018] Embodiment 2: the preparation of alfuzosin hydrochloride
[0019] In a 3000 ml three-necked flask with mechanical stirring, add 1600 ml of DMF (N, N-dimethylformamide) and 98 ml of pyridine, stir with 5 g of DMAP, cool to 0 ° C, add 88 g of N-methyl Propylenediamine and 104.5 grams of 2-tetrahydrofurancarboxylic acid were reacted at room temperature for 20 hours, and 245.5 grams of 2-chloro-4-amino-6,7-dimethoxyquinazoline were added. Control the temperature at 35-40°C and react for 14 hours. After completion of the reaction, wash with water (1000 ml × 2), 5% NaHCO 3 Wash with 800 ml of aqueous solution, wash with 800 ml of saturated saline, and wash with anhydrous Na 2 SO 4 dry. After evaporating the solvent under reduced pressure, dissolve it with 1500 ml of absolute ethanol, add 180 ml of absolute ethanol-hydrogen chloride, stir evenly, place to crystallize, filter with suction, and dry to obtain 226 grams of white crystalline solid, which is the fine product of ...
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